CN102659099A - Preparation method of anisotropic graphene foam - Google Patents
Preparation method of anisotropic graphene foam Download PDFInfo
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- CN102659099A CN102659099A CN201210171707XA CN201210171707A CN102659099A CN 102659099 A CN102659099 A CN 102659099A CN 201210171707X A CN201210171707X A CN 201210171707XA CN 201210171707 A CN201210171707 A CN 201210171707A CN 102659099 A CN102659099 A CN 102659099A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 71
- 239000006260 foam Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 56
- 239000006185 dispersion Substances 0.000 claims abstract description 26
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 25
- 239000010439 graphite Substances 0.000 claims abstract description 25
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000007791 liquid phase Substances 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000013543 active substance Substances 0.000 claims description 7
- 230000006872 improvement Effects 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 230000005855 radiation Effects 0.000 claims description 5
- 230000003019 stabilising effect Effects 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- 230000002829 reductive effect Effects 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 235000010378 sodium ascorbate Nutrition 0.000 claims description 2
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 claims description 2
- 229960005055 sodium ascorbate Drugs 0.000 claims description 2
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000004094 surface-active agent Substances 0.000 abstract description 2
- 239000011814 protection agent Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 15
- 230000008569 process Effects 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 230000003252 repetitive effect Effects 0.000 description 3
- 238000005201 scrubbing Methods 0.000 description 3
- YZHUMGUJCQRKBT-UHFFFAOYSA-M sodium chlorate Chemical compound [Na+].[O-]Cl(=O)=O YZHUMGUJCQRKBT-UHFFFAOYSA-M 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229920003081 Povidone K 30 Polymers 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000006262 metallic foam Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 229940001516 sodium nitrate Drugs 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002238 carbon nanotube film Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005520 electrodynamics Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
Images
Abstract
The invention relates to a preparation method of anisotropic graphene foam. The method comprises the following steps of: (1) preparing graphite oxide; (2) preparing a graphene oxide dispersion solution, namely dispersing the graphite oxide prepared in the step (1) into a solution to prepare the graphene oxide dispersion solution; (3) preparing a graphene dispersion solution, namely adding a surfactant or a reducing agent with certain surface activity into the dispersion solution of the step (2) to be used as a protection agent; and preparing the graphene dispersion solution through chemical liquid-phase reduction; and (4) preparing the anisotropic graphene foam: damaging a previous graphene stable system to self-assemble the graphene into the anisotropic graphene foam. The graphene foam prepared by the method is composed of at least one layer of graphene structure unit and has anisotropies of a structure and a property in a graphene growth direction and in a direction which is vertical to the growth direction; the specific surface area of the anisotropic graphene foam is 200-2000 m<2>/g; and the heat conductivity difference in the graphene growth direction and in the direction which is vertical to the growth direction reaches to two magnitudes.
Description
Technical field
The present invention relates to a kind of preparation method of anisotropy grapheme foam, belong to new material technology field.
Background technology
New material industry has become one of new high-tech industry with fastest developing speed since getting into 21 century, also is the technological highland that various countries competitively capture.The research that with the Graphene is the new carbon of representative obtains a series of important breakthroughs; On October 5th, 2010, the physicist An Deliehaimu of Univ Manchester UK (Andre Geim) professor and Constantine Nuo Woxiaoluofu (Konstantin Novoselov) teach because of the research of being engaged in Graphene and have disclosed its character and obtain Nobel Prize in physics in 2010.
Graphene is the carbon simple substance of neatly being arranged and forming by hexagonal lattice by carbon atom, and structure is highly stable.Research shows that the electronic mobility of Graphene is higher, can do electrode thinlyyer, more transparent, good electrical conductivity and to the high-permeability of light make its in fields such as liquid-crystal display and solar cells unique advantage.Graphene film has the field emission characteristic of comparing mutually with carbon nano-tube film, has very application prospects at aspects such as semiconducter device and FPD; Because its unique two-dirnentional structure and excellent crystallography quality for the quantum electrodynamics phenomenon Study provides ideal platform, have important theoretical research and are worth.In addition, after Graphene and plastics are compound, can make it become conductor and improve its mechanical property and thermotolerance.The compounded novel material of Graphene and plastics, light and handy and firm, can be applicable to the vehicles such as man-made satellite of new generation, aircraft and automobile.Thereby Graphene is expected to obtain to use widely in fields such as high-performance nano electron device, matrix material, gas sensor and energy storages.
Graphene and associated materials thereof be because its excellent electricity, calorifics and mechanical property, caused the extensive concern of community of physicists, material educational circles.Preparation method of graphene comprises: micromechanics partition method, epitaxy method-Epitaxial Growth, heating SiC method, chemical Vapor deposition process, chemical reduction method etc.Graphene is the unit molecule planar materials, is a kind of two-dirnentional structure, and it is still rarely found to adopt this two-dirnentional structure material to construct the document and the patent of said three-dimensional body material.2011, (associating) the laboratory Cheng Huiming of Shenyang Materials science country of metal institute of the Chinese Academy of Sciences, a literary talent led research team to prepare Graphene said three-dimensional body material (Chen ZP, Ren WC; Gao LB, Liu BL, Pei SF; Cheng HM, Three-dimensional flexible and conductive interconnected graphene networks grown by chemical vapour deposition.Nature Material, 2011; 10,424 – 428).The method that they adopt is chemical vapour deposition: with foamed metals such as copper or nickel is body material, and the monolayer carbon atom invests the surface of foamed metal, like this, and the structure that Graphene body material has intactly duplicated foamed metal; After etching away matrix metal materials such as copper or nickel, just obtained this Graphene said three-dimensional body material.This method has adopted the method for a kind of similar hard template (is template with the metal foam) to prepare three-dimensional grapheme foam, but the method for chemical vapour deposition, the difficult control of processing condition; Need very personnel's accuracy controlling of specialty; And need be with foamed metals such as copper or nickel as hard template, the preparation technology of this hard template is comparatively complicated, and price is more expensive; And remove in the process of hard template in etching, possibly form some influences the Graphene performance defect.Still seldom have at present and adopt the method for self-assembly to prepare grapheme foam; This method is for hard template method; Self-assembly method preparation technology is simpler; The pressure that does not also have environmental pollution, and this method can obtain having the grapheme foam of anisotropic character, and significant for the characteristic of performance Graphene.
Summary of the invention
The objective of the invention is to overcome the deficiency in the existing graphene preparation method; And a kind of preparation method of anisotropy grapheme foam is provided; This method does not adopt body materials such as foamed metal; Need not remove the metal foam template, have with low cost, simple, advantage such as be produced on a large scale.
For realizing the object of the invention, technical scheme of the present invention is:
A kind of preparation method of anisotropy grapheme foam, this method may further comprise the steps:
(1) preparation graphite oxide;
(2) preparation graphene oxide dispersion liquid: the graphite oxide of preparation in the step (1) is dispersed in the solution preparation graphene oxide dispersion liquid;
(3) add tensio-active agent or itself have the active reductive agent of certain surface in the dispersion liquid preparation Graphene dispersion liquid: to step 2), through chemical liquid phase reduction preparation Graphene dispersion liquid as protective material;
(4) preparation anisotropy grapheme foam: destroy original Graphene stabilising system, make Graphene be self-assembled into anisotropic foam.
In a preferred embodiment of the present invention; Preparation has the method for anisotropy grapheme foam; In the step 1), the method for preparing graphite oxide is a kind of in Staudenmaier method or the Hofmann method of Brodie method, improvement of Hummers method, improvement Hummers method, improvement.
In a preferred embodiment of the present invention, the described method for preparing the anisotropy grapheme foam, step 2) in, said solution is water or ethanol.
In a preferred embodiment of the present invention, the described method for preparing the anisotropy grapheme foam, step 2) in, what said graphite oxide disperseed employing is ultrasonic, or mechanical stirring or both common implementings.
In a preferred embodiment of the present invention, the described method for preparing the anisotropy grapheme foam, in the step 3), described tensio-active agent is one or more the mixture in polyoxyethylene glycol, Vinylpyrrolidone polymer or the ZX-I.
In a preferred embodiment of the present invention; The described method for preparing the anisotropy grapheme foam; In the step 3), described reductive agent is one or more the mixture in L-halfcystine, Hydrocerol A, Trisodium Citrate, xitix or the sodium ascorbate.
In a preferred embodiment of the present invention, the described method for preparing the anisotropy grapheme foam, in the step 4), what destroy that the method for original Graphene stabilising system adopts is one in heating, radiation or the flocculation or both above common implementings.
The present invention compares with existing preparation method; Its advantage and positively effect are: the method for preparing the anisotropy grapheme foam disclosed by the invention is to be presoma with the graphene oxide dispersion liquid; Through reduction to graphene oxide; Preparation Graphene dispersion liquid destroys original Graphene stabilising system through methods such as heating, radiation or flocculations again, and Graphene is become non-wetting ability by wetting ability; Thereby be self-assembled into grapheme foam, this grapheme foam has bigger specific surface area (200-2000m
2/ g); Graphene is in the process of assembling; Owing to reasons such as migration resistance; Have anisotropic characteristic, its along the Graphene direction of growth and perpendicular to producer to the thermal conductivity difference reach two one magnitude, this is that chemical Vapor deposition process is not accomplished; Thermal conductivity along the Graphene direction of growth can reach 200W/m.k, and perpendicular to producer to thermal conductivity have only 0.5W/m.k.
Description of drawings
Sample the photo in synthetic liquid of Fig. 1 (a) for adopting instance 1 preparation, Fig. 1 (b) is the photo after the sample of instance 1 preparation takes out.This grapheme foam is cylindric, and diameter is about 3cm, highly is 3.5cm, and its specific surface area is 2012m
2/ g is 211W/m.k along the thermal conductivity of the Graphene direction of growth, perpendicular to producer to thermal conductivity be 0.5W/m.k.
Fig. 2 (a) is for adopting the sample photo of instance 2 preparations, and this grapheme foam is cylindric, and there is depression at the middle part, and diameter is about 2.8cm, highly about 4cm.Fig. 2 (b) is the sem photograph of this sample, can find out, this grapheme foam is tangible anisotropy, and its specific surface area is 536m
2/ g is 120W/m.k along the thermal conductivity of the Graphene direction of growth, perpendicular to producer to thermal conductivity be 0.3W/m.k.
Fig. 3 (a) is the sem photograph of the sample of employing instance 3 preparations; Can find out that therefrom this grapheme foam is tangible laminate structure, this grapheme foam has formed slight crack in the exsiccant process; Fig. 3 (b) is the photo of sample after amplifying; Can find out obviously that this Graphene tiles to a direction, also present tangible anisotropy, its specific surface area is 365m
2/ g is 63W/m.k along the thermal conductivity of the Graphene direction of growth, perpendicular to producer to thermal conductivity be 0.8W/m.k.
Fig. 4 (a) can find out therefrom that for the sem photograph of the sample of employing instance 4 preparations this sample is strip.Because the precursor concentration of this grapheme foam is lower, so the grapheme foam of preparation gained is smaller.Fig. 4 (b) is the sem photograph of this sample end face, can find out grapheme foam anisotropic character highly significant, and its specific surface area is 536m
2/ g is 870W/m.k along the thermal conductivity of the Graphene direction of growth, perpendicular to producer to thermal conductivity be 0.7W/m.k.
Fig. 5 (a) and (b) are the sem photograph of the grapheme foam different angles of employing instance 5 preparations; Therefrom can find out; (a) be Graphene tiling direction, and (b) be the side elevational view of tiling direction, can find out that this grapheme foam has and be tangible laminate structure; Have anisotropic character, its specific surface area is 1036m
2/ g is 96W/m.k along the thermal conductivity of the Graphene direction of growth, perpendicular to producer to thermal conductivity be 0.5W/m.k.
Embodiment
Below in conjunction with specific embodiment, further specify the present invention.
Adopt the Hummers legal system to be equipped with graphite oxide: in ice bath, 10g Graphite Powder 99 and the 5g SODIUMNITRATE and the 230mL vitriol oil to be mixed slow adding 30g KMnO in the stirring
4It is transferred in 35 ° of C water-baths reaction 30 minutes, progressively adds the 460mL deionized water again, when temperature rises to 98 ℃ of continued reactions 40 minutes, mixture becomes glassy yellow by brown, further thin up, and to use massfraction be 30% H
2O
2Solution-treated, the unreacted permanganic acid that neutralizes, centrifuging and repetitive scrubbing filter cake promptly obtain graphite oxide with its vacuum-drying at last; Graphite oxide is ground, preparation 2mg/mL suspension-s 100mL in water, supersound process 30min obtains the stable graphene oxide colloidal suspensions of homogeneous; Add tensio-active agent Vinylpyrrolidone polymer (PVP-K30) 0.2g, ultrasonic dissolution adds 1g L-halfcystine, obtains stable Graphene dispersion liquid; This dispersion liquid is heated to 95 ℃ continues reaction 2 hours, after the cooling, can obtain grapheme foam.
Embodiment 2
Adopt the Staudenmaier legal system to be equipped with graphite oxide: the mixed solution of at first in there-necked flask, preparing the nitrosonitric acid (27ml) and the vitriol oil (87.5ml); Then this there-necked flask is put in ice bath and cooled off; The 5g Graphite Powder 99 is under agitation slowly gone into subsequently (noting: need this there-necked flask is put in the ice bath always,, avoid blast) with slowed down reaction speed; 55g VAL-DROP is added in the above-mentioned reaction system; Continued stirring reaction 96 hours, reaction obtains graphite oxide with the reaction mixture filtration washing after finishing; Graphite oxide is ground, preparation 2mg/mL suspension-s 100mL in water, supersound process 30min obtains the stable graphene oxide colloidal suspensions of homogeneous; Add tensio-active agent ZX-I 0.2g, ultrasonic dissolution adds the 2g Trisodium Citrate; This dispersion liquid is heated to 95 ℃ of reactions after 4 hours, after the cooling, can obtains grapheme foam rapidly.
Embodiment 3
Adopt the Brodie method of improvement to prepare graphite oxide: in ice bath, 10g Graphite Powder 99 and 85g VAL-DROP and 200mL nitrosonitric acid are mixed, stirring is 24 hours under the room temperature.After reaction finishes, centrifuging and repetitive scrubbing filter cake, purifying promptly obtains graphite oxide with its vacuum-drying at last.Graphite oxide is ground, preparation 2mg/mL suspension-s 100mL in water, supersound process 30min obtains the stable graphene oxide colloidal suspensions of homogeneous.Add xitix 2g, ultrasonic dissolution obtains stable Graphene dispersion liquid.With this Graphene dispersion liquid microwave radiation reaction 15min, cool off and to obtain grapheme foam in back 12 hours.
Embodiment 4
Adopt the Hummers legal system to be equipped with graphite oxide: in ice bath, 10g Graphite Powder 99 and the 5g SODIUMNITRATE and the 230mL vitriol oil to be mixed slow adding 30g KMnO in the stirring
4, it is transferred in 35 ° of C water-baths reaction 30 minutes, progressively add the 460mL deionized water again, when temperature rises to 98 ℃ of continued reactions 40 minutes, mixture becomes glassy yellow by brown, further thin up, and to use massfraction be 30% H
2O
2Solution-treated, the unreacted permanganic acid that neutralizes, centrifuging and repetitive scrubbing filter cake promptly obtain graphite oxide with its vacuum-drying at last; Graphite oxide is ground, preparation 0.5mg/mL suspension-s 100mL in ethanol, supersound process 30min obtains the stable graphene oxide colloidal suspensions of homogeneous; Add tensio-active agent Vinylpyrrolidone polymer (PVP-K30) 0.2g, ultrasonic dissolution adds 1g L-halfcystine, obtains stable Graphene dispersion liquid; This dispersion liquid is added flocculation agent aluminum chloride 0.1g, can obtain grapheme foam after 12 hours.
Embodiment 5
Adopt the Staudenmaier legal system to be equipped with graphite oxide: the mixed solution of at first in there-necked flask, preparing the nitrosonitric acid (27ml) and the vitriol oil (87.5ml); Then this there-necked flask is put in ice bath and cooled off; The 5g Graphite Powder 99 is under agitation slowly gone into subsequently (noting: need this there-necked flask is put in the ice bath always,, avoid blast) with slowed down reaction speed; 55g VAL-DROP is added in the above-mentioned reaction system; Continued stirring reaction 96 hours, reaction obtains graphite oxide with the reaction mixture filtration washing after finishing; Graphite oxide is ground, preparation 2mg/mL suspension-s 100mL in water, ultrasonic double stir process 60min obtains the stable graphene oxide colloidal suspensions of homogeneous; Add surfactant polyethylene 0.2g, ultrasonic dissolution adds 2g L-halfcystine, obtains stable Graphene dispersion liquid; With this dispersion liquid microwave radiation reaction 30min, slowly after the cooling, can obtain grapheme foam.
Claims (7)
1. the preparation method of an anisotropy grapheme foam is characterized in that, this method may further comprise the steps:
(1) preparation graphite oxide;
(2) preparation graphene oxide dispersion liquid: the graphite oxide of preparation in the step (1) is dispersed in the solution preparation graphene oxide dispersion liquid;
(3) add tensio-active agent or itself have the active reductive agent of certain surface in the dispersion liquid preparation Graphene dispersion liquid: to step 2), through chemical liquid phase reduction preparation Graphene dispersion liquid as protective material;
(4) preparation anisotropy grapheme foam: destroy original Graphene stabilising system, make Graphene be self-assembled into anisotropic foam.
2. preparation according to claim 1 has the method for anisotropy grapheme foam; It is characterized in that; In the step 1), the method for preparing graphite oxide is a kind of in Staudenmaier method or the Hofmann method of Brodie method, improvement of Hummers method, improvement Hummers method, improvement.
3. the method for preparing the anisotropy grapheme foam according to claim 1 is characterized in that step 2) in, said solution is water or ethanol.
4. the method for preparing the anisotropy grapheme foam according to claim 1 is characterized in that step 2) in, what said graphite oxide disperseed employing is ultrasonic, or mechanical stirring or both common implementings.
5. the method for preparing the anisotropy grapheme foam according to claim 1 is characterized in that, in the step 3), described tensio-active agent is one or more the mixture in polyoxyethylene glycol, Vinylpyrrolidone polymer or the ZX-I.
6. the method for preparing the anisotropy grapheme foam according to claim 1; It is characterized in that; In the step 3), described reductive agent is one or more the mixture in L-halfcystine, Hydrocerol A, Trisodium Citrate, xitix or the sodium ascorbate.
7. the method for preparing the anisotropy grapheme foam according to claim 1 is characterized in that, in the step 4), what destroy that the method for original Graphene stabilising system adopts is one in heating, radiation or the flocculation or both above common implementings.
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| CN103407994A (en) * | 2013-07-17 | 2013-11-27 | 苏州艾特斯环保材料有限公司 | Method for reducing graphene oxide |
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| CN101941693A (en) * | 2010-08-25 | 2011-01-12 | 北京理工大学 | Graphene aerogel and preparation method thereof |
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