CN101837972A - Graphene three-dimensional structure and preparation method thereof - Google Patents
Graphene three-dimensional structure and preparation method thereof Download PDFInfo
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- CN101837972A CN101837972A CN 201010187509 CN201010187509A CN101837972A CN 101837972 A CN101837972 A CN 101837972A CN 201010187509 CN201010187509 CN 201010187509 CN 201010187509 A CN201010187509 A CN 201010187509A CN 101837972 A CN101837972 A CN 101837972A
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Abstract
The invention discloses a three-dimensional structure constructed by using graphene as base units and a preparation method thereof. The graphene three-dimensional structure is formed by stacking and assembling graphene, the shape of the graphene three-dimensional structure is a similar cylinder or a polygonal prism, and the volume of the graphene three-dimensional structure is 0.1-100cm<3>. The graphene three-dimensional structure can contain water, methanol, ethanol, glycol and mixture molecules thereof, and can contain Li<+>, Na<+>, K<+>, Ag<+>, Ca<2+>, Ba<2+>, Mg<2+>, Ni<2+>, Co<2+>, Cu<2+>, Mn<2+>, Cd<2+>, Zn<2+>, Pb<2+>, Pt<2+>, Pd<2+>, Rh<2+>, Al<3+>, Fe<3+>, Au<3+>, Ru<3+> and Pt<4+> metal ions. The graphene three-dimensional structure has rich network space which can be used for filling Ni, Co, Cu, Mn, Fe, Au, Ag, Pt and Ru as well as alloy nanoparticles thereof, can be used for filling polypyrrole, polyaniline, polyacrylic acid, polythiophene, polyacrylamide and polyvinyl alcohol polymers, and can be used for filling protein, amino acid, sugar and enzyme biological molecules.
Description
Technical field
The present invention relates to graphene three-dimensional structure and preparation method.
Background technology
By the Graphene (graphene) of monolayer carbon atomic building, the physicochemical property with a series of excellences, as the electricity of excellence lead, mechanical property, huge specific surface area etc.Single-layer graphene can be used for field-effect transistor, high-frequency element, super microprocessor and single-molecule detection device etc.And be the three-dimensional structure that elementary cell constitutes by Graphene, as film and bulk material, might be applied to field of functional materials such as controlled Breathable films, anisotropy ion-conducting material, ultracapacitor, lithium ion battery, molecule storage, electrochemical sensing, fuel cell, energy catalysis; Or field of compound material such as polymkeric substance, pottery and metal.
In order to realize the preparation of graphene three-dimensional structure, must possess competent Graphene raw material.The graphite oxide reduction method can satisfy this requirement, and this method also can provide graphene oxide (graphene oxide) in a large number.Graphene oxide has a large amount of oxygen-containing functional groups and excellent dispersiveness, therefore has good film-forming properties.At present, the preparation graphene oxide film mainly comprises three kinds of methods: the one, generate the graphene oxide filter cake by filtering, and make [Dikin, et al.Nature, 2007,448,457.] after the drying; The 2nd, by the evaporation acquisition solid film [Cai, et al.Adv.Function.Mater., 2008,20,1706] of solvent in the graphene oxide solution; The 3rd, utilize functional group's self-assembly of graphene oxide, as L B film [Li, et al.Nat.Nanotechnol., 2008,3,538.].And for Graphene, because the removal significantly of its surperficial functional group increases the technology difficulty of self-assembly film forming, so more feasible film is the former two.It is pointed out that the rare film forming bonding force with Graphene of graphite oxide is different, the former mainly relies on hydrogen bond and electrostatic interaction; And the latter mainly relies on π-π effect and is aided with a spot of electrostatic force.Functional group in the graphene oxide can be used for connecting materials such as ion, polymer and carbon nanotube, therefore can prepare corresponding compound oxidizing graphene film.Still need further to explore and prepare similar compound graphene film.The conductive capability of graphene oxide is than low at least 2 orders of magnitude of Graphene.Therefore, in application facet such as electricity storage and conversions, graphene film has more advantage than graphene oxide film.Research report at graphene three-dimensional structure still rests on this scope of film shape at present, and the preparation of block three-dimensional structure is still a challenging research topic.Exploitation blocky graphite alkene three-dimensional structure material has important theory and practical significance.
Summary of the invention
Technical problem: the objective of the invention is to develop the Graphene self-assembling technique, the preparation graphene three-dimensional structure.On this basis, realization is to the adjusting of graphene layer spacing in the graphene three-dimensional structure; Be implemented in and fill ion, molecule and nanoparticle in the graphene layer.
Technical scheme: graphene three-dimensional structure of the present invention specifically comprises following content:
Graphene three-dimensional structure is to be elementary cell with the Graphene, under the temperature and pressure of determining, forms by metal ion bridging self-assembly; This Graphene is individual layer or 2-10 layer structure, and hydroxyl, epoxy and carboxylic acid are contained in the Graphene surface, or any one or a few oxygen-containing functional group wherein, and the ratio of metal ion and Graphene is at 0.1%-100%.
Comprise Li in the graphene three-dimensional structure
+, Na
+, K
+, Ag
+, Ca
2+, Ba
2+, Mg
2+, Ni
2+, Co
2+, Cu
2+, Mn
2+, Cd
2+, Zn
2+, Pb
2+, Pt
2+, Pd
2+, Rh
2+, Al
3+, Fe
3+, Au
3+, Ru
+, Pt
4+Metal ion.
Comprise water, methyl alcohol, ethanol, ethylene glycol and composition thereof molecule in the graphene three-dimensional structure.Can fill out Ni, Co, Cu, Mn, Fe, Au, Ag, Pt, Ru and alloy nano particle thereof in the graphene three-dimensional structure.Can fill polypyrrole, polyaniline, polyacrylic acid, Polythiophene, polyacrylamide, polyvinyl alcohol polymer in the graphene three-dimensional structure.Can fill albumen, amino acid, sugar and enzyme biomolecules in the graphene three-dimensional structure.
The preparation method of graphene three-dimensional structure may further comprise the steps:
1) use the Hummers method, Brodie method or Staudenmaier legal system are equipped with graphite oxide,
2) graphite oxide is placed water or ethanol or the two mixing solutions, the mass ratio of graphite oxide and solution is 1/100-1/10000, and the supersound process through 25min～35min obtains graphene oxide solution,
3) graphene oxide solution is poured in the withstand voltage and resistant to elevated temperatures reaction vessel, added Ca
2+, Ba
2+, Mg
2+, Ni
2+, Co
2+, Cu
2+, Mn
2+, Cd
2+, Zn
2+, Pb
2+, Pt
2+, Pd
2+Or Rh
2+Divalent ion solution; Or above-mentioned ionic mixing solutions; Or above-mentioned ion and Li
+, Na
+, K
+, Ag
+, Al
3+, Fe
3+, Au
3+, Ru
3+, Pt
4+One or more ion mixing solutionss wherein,
4) scope of regulator solution pH is 1～14,
5) control reaction temperature is at 70～260 ℃, and pressure is at 0.1～20MPa, and the reaction times makes graphene three-dimensional structure at 0.5～240h,
6) graphene three-dimensional structure is placed deionized water, adds Ni, Co, Cu, Mn, Fe, Au, Ag, Pt, Ru or its alloy nano particle, through the 1-48h exchange, the nano-particles filled in the solution in graphene three-dimensional structure,
7) graphene three-dimensional structure is placed deionized water, or in the phosphate buffer soln, add albumen, amino acid, sugar or enzyme biomolecules,, the biomolecules in the solution is filled in the graphene three-dimensional structure through the 1-48h exchange.
Beneficial effect: the present invention proposes the notion of graphene three-dimensional structure, a kind of method for preparing graphene three-dimensional structure is provided, have following characteristics and advantage:
(1) the present invention utilizes water to do the reductive agent redox graphene and obtains Graphene, and this Graphene surface keeps a certain amount of hydroxyl and epoxy group(ing), and this provides available functional group for self-assembly.
(2) it is interconnection to utilize bivalent ions bridging effect to make between the Graphene, is assembled into three-dimensional structure.
(3) by adjusting pH value, or control reaction pressure or temperature, the interlamellar spacing of regulating graphene layer in the graphene three-dimensional structure.
(4) comprise water or alcohol solvent in the layer in the graphene three-dimensional structure, can make things convenient for other material to fill.
Prepared graphene three-dimensional structure of the present invention can be used as electrode materials and is applied in solar cell, fuel cell, lithium ion battery and the ultracapacitor; Can be used as packing material and be used for matrix material.
Embodiment
(1) use the Hummers method, Brodie method or Staudenmaier legal system are equipped with graphite oxide.
(2) graphite oxide is placed water or ethanol or the two mixing solutions, the mass ratio of graphite oxide and solution is 1/100-1/10000, and the supersound process of generally passing through general 30min obtains graphene oxide solution.
(3) graphene oxide solution is poured in the reaction vessel of withstand voltage (peak pressure is 50MPa) and high temperature resistant (top temperature is 300 ℃), added Ca
2+, Ba
2+, Mg
2+, Ni
2+, Co
2+, Cu
2+, Mn
2+, Cd
2+, Zn
2+, Pb
2+, Pt
2+, Pd
2+Or Rh
2+Divalent ion solution; Or above-mentioned ionic mixing solutions; Or above-mentioned ion and Li
+, Na
+, K
+, Ag
+, Al
3+, Fe
3+, Au
3+, Ru
3+, Pt
4+One or more ion mixing solutionss wherein.
(4) scope of regulator solution pH is 1～14.
(5) control reaction temperature is at 70～260 ℃, and pressure is at 0.1～20MPa, and the reaction times is at 0.5～240h.Make graphene three-dimensional structure.
(6) graphene three-dimensional structure is placed deionized water, adds Ni, Co, Cu, Mn, Fe, Au, Ag, Pt, Ru or its alloy nano particle, through the 1-48h exchange, the nano-particles filled in the solution in graphene three-dimensional structure.
(7) graphene three-dimensional structure is placed deionized water, or in the phosphate buffer soln, add albumen, amino acid, sugar or enzyme biomolecules,, the biomolecules in the solution is filled in the graphene three-dimensional structure through the 1-48h exchange.
Below in conjunction with accompanying drawing and example to this experiment be elaborated (example is the concrete operations of illustrative experiment, any qualification is not carried out in invention):
Graphite oxide used in the present invention is to be raw material with the crystalline flake graphite, adopts the preparation of Hummers method.
Embodiment 1 gets the 30mg graphite oxide and is dissolved in the 45mL water, and supersound process 60min transfers to solution on the magnetic stirring apparatus then and stirs, and adds 4.16mg CaCl
2, behind the stirring 30min, place the 50mL reactor, preserve 12h down at 150 ℃.Obtain Ca after the cooling
2+The cylindrical graphene three-dimensional structure of ion bridging.
Embodiment 2 gets the 30mg graphite oxide and is dissolved in the 45mL water, and supersound process 60min transfers to solution on the magnetic stirring apparatus then and stirs, and adds 4.16mg CaCl
2, behind the stirring 30min, add NaOH solution, regulate pH to 10.Then solution is moved in the 50mL reactor, preserve 12h down at 150 ℃.Obtain Ca after the cooling
2+The cylindrical graphene three-dimensional structure of ion bridging.
Embodiment 3 gets the 30mg graphite oxide and is dissolved in the 45mL water, and supersound process 60min transfers to solution on the magnetic stirring apparatus then and stirs, and adds 2.28mg BaCl
2, behind the stirring 30min, place the 50mL reactor, preserve 12h down at 150 ℃.Obtain Ba after the cooling
2+The cylindrical graphene three-dimensional structure of ion bridging.
Embodiment 4 gets the 30mg graphite oxide and is dissolved in the 45mL water, and supersound process 60min transfers to solution on the magnetic stirring apparatus then and stirs, and adds 3.31mg NiCl
2, behind the stirring 30min, place the 50mL reactor, preserve 12h down at 150 ℃.Obtain Ni after the cooling
2+The cylindrical graphene three-dimensional structure of ion bridging.
Embodiment 4 gets the 30mg graphite oxide and is dissolved in the 45mL water, and supersound process 60min transfers to solution on the magnetic stirring apparatus then and stirs, and adds 3.28mg CoCl
2, behind the stirring 30min, place the 50mL reactor, preserve 12h down at 150 ℃.Obtain Ni after the cooling
2+The cylindrical graphene three-dimensional structure of ion bridging.
Embodiment 5 gets the 30mg graphite oxide and is dissolved in the 45mL water, and supersound process 60min transfers to solution on the magnetic stirring apparatus then and stirs, and adds 4.16mg CaCl
2With 1mg LiCl, behind the stirring 30min, place the 50mL reactor, preserve 12h down at 150 ℃.Contained Ca after the cooling simultaneously
2+And Li
+Graphene three-dimensional structure.
Embodiment 6 is Ca
2+It is the gold size solution of 0.1mg/mL that the graphene three-dimensional structure of ion bridging (preparation method sees embodiment 1) places concentration, leaves standstill 24h, obtains the graphene three-dimensional structure that the gold nano ion is filled.
Embodiment 7 is Ca
2+It is the pyrrole monomer solution of 0.1mg/mL that the graphene three-dimensional structure of ion bridging (preparation method sees embodiment 1) places concentration, leave standstill 24h, add the 0.5mg ammonium persulfate then, polymerization 24h under condition of ice bath obtains the graphene three-dimensional structure that polypyrrole is filled.
Embodiment 8 is Ca
2+It is the horseradish peroxidase solution of 0.1mg/mL that the graphene three-dimensional structure of ion bridging (preparation method sees embodiment 1) places concentration, leaves standstill 24h, obtains the graphene three-dimensional structure that horseradish peroxidase is filled.
Embodiment 9 is Ni
2+The graphene three-dimensional structure of ion bridging (preparation method sees embodiment 4) places the aqueous solution, slowly drips the NaBH of 0.1M then
4Solution obtains the graphene three-dimensional structure that nickel nano particle is filled.
Embodiment 10 uses pressure sintering, at 220 ℃, under the 20MPa graphene three-dimensional structure is pressed into graphene film.
Claims (7)
1. a graphene three-dimensional structure is characterized in that graphene three-dimensional structure is is elementary cell with the Graphene, under the temperature and pressure of determining, forms by metal ion bridging self-assembly; This Graphene is individual layer or 2-10 layer structure, and hydroxyl, epoxy and carboxylic acid are contained in the Graphene surface, or any one or a few oxygen-containing functional group wherein, and the ratio of metal ion and Graphene is at 0.1%-100%.
2. according to the described graphene three-dimensional structure of claim l, it is characterized in that comprising in the graphene three-dimensional structure Li
+, Na
+, K
+, Ag
+, Ca
2+, Ba
2+, Mg
2+, Ni
2+, Co
2+, Cu
2+, Mn
2+, Cd
2+, Zn
2+, Pb
2+, Pt
2+, Pd
2+, Rh
2+, Al
3+, Fe
3+, Au
3+, Ru
3+, Pt
4+Metal ion.
3. graphene three-dimensional structure according to claim 1 is characterized in that comprising in the graphene three-dimensional structure water, methyl alcohol, ethanol, ethylene glycol and composition thereof molecule.
4. graphene three-dimensional structure according to claim 1 is characterized in that can filling Ni, Co, Cu, Mn, Fe, Au, Ag, Pt, Ru and alloy nano particle thereof in the graphene three-dimensional structure.
5. graphene three-dimensional structure according to claim 1 is characterized in that can filling polypyrrole, polyaniline, polyacrylic acid, Polythiophene, polyacrylamide, polyvinyl alcohol polymer in the graphene three-dimensional structure.
6. graphene three-dimensional structure according to claim 1 is characterized in that can filling in the graphene three-dimensional structure albumen, amino acid, sugar and enzyme biomolecules.
7. the preparation method of a graphene three-dimensional structure as claimed in claim 1 is characterized in that this method may further comprise the steps:
1) use the Hummers method, Brodie method or Staudenmaier legal system are equipped with graphite oxide,
2) graphite oxide is placed water or ethanol or the two mixing solutions, the mass ratio of graphite oxide and solution is 1/100-1/10000, and the supersound process through 25min～35min obtains graphene oxide solution,
3) graphene oxide solution is poured in the withstand voltage and resistant to elevated temperatures reaction vessel, added Ca
2+, Ba
2+, Mg
2+, Ni
2+, Co
2+, Cu
2+, Mn
2+, Cd
2+, Zn
2+, Pb
2+, Pt
2+, Pd
2+Or Rh
2+Divalent ion solution; Or above-mentioned ionic mixing solutions; Or above-mentioned ion and Li
+, Na
+, K
+, Ag
+, Al
3+, Fe
3+, Au
3+, Ru
3+, Pt
4+One or more ion mixing solutionss wherein,
4) scope of regulator solution pH is 1～14,
5) control reaction temperature is at 70～260 ℃, and pressure is at 0.1～20MPa, and the reaction times makes graphene three-dimensional structure at 0.5～240h,
6) graphene three-dimensional structure is placed deionized water, adds Ni, Co, Cu, Mn, Fe, Au, Ag, Pt, Ru or its alloy nano particle, through the 1-48h exchange, the nano-particles filled in the solution in graphene three-dimensional structure,
7) graphene three-dimensional structure is placed deionized water, or in the phosphate buffer soln, add albumen, amino acid, sugar or enzyme biomolecules,, the biomolecules in the solution is filled in the graphene three-dimensional structure through the 1-48h exchange.
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