CN102660740B - Graphene and metal nanoparticle composite film preparation method - Google Patents
Graphene and metal nanoparticle composite film preparation method Download PDFInfo
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Abstract
The invention relates to a graphene and metal nanoparticle composite film preparation method. The graphene and metal nanoparticle composite film mainly comprises a first graphene film layer (1), a second graphene film layer (3), a third graphene film layer (5), a first metal nanoparticle film layer (2) and a second metal nanoparticle film layer (4). The graphene film layers and the metal nanoparticle film layers are overlapped alternatively to form the graphene and metal nanoparticle composite film and then are composited with a base material (6) into a whole serving as a molecular Raman signal detection substrate or a transparent efficacy-enhancement solar cell electrode. The graphene and metal nanoparticle composite film has characteristics of transparency, conductivity, surface plasma enhancement and the like, can be used as the molecular signal detection substrate or the transparent solar cell electrode having a trapping effect, and is expected to be applied to surface Raman scattering enhancement, photovoltaic efficacy enhancement or other related fields widely.
Description
Technical field
The invention belongs to nano material preparing technical field, specifically the preparation method of a kind of Graphene and metal nanoparticle laminated film.
Background technology
In recent years, Graphene and metal nanoparticle, because the characteristics such as its unique optics, electricity, mechanics and katalysis and physiologically acceptable have caused interest widely in nanosecond science and technology field, have huge application prospect in electron transport device, electrode capactitance device, sensor, Single Molecule Detection, photovoltaic synergy and prepare composite.
The special property of metal nanoparticle, if surface plasma excimer effect is because nano grain surface unbound electron is subject to electric field component excitation in incident electromagnetic wave (or incident light), interacts and produce, and forms surface plasma excimer.This surface plasma excimer can produce amplification higher than incident electromagnetic wave (or incident light)
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local electric field intensity doubly.Because the high strength of electric field of local is of value to the amplification of unit molecule Raman detection signal and improves the specific absorption of solar device to incident light, and once becoming the hot technology in biomolecule detection and photovoltaic synergy field.In field of biological detection, research is found, when metal nanoparticle is coupled near generation mutually, can change the optical property of nano material, and can further improve the strength of electric field of metal nanoparticle surface local, thereby improve molecule Raman detection strength of signal, yet the minimum distance between metal nanoparticle (10 nanometers are following) is comparatively difficult aspect nano material technology of preparing, by traditional nanoimprinting technology, generally can only accomplish the above distance of 10 nanometer, so the coupling distance of accurately controlling between nano particle is one of a great problem of field of nanometer technology.In emerging photovoltaic field, metal nanoparticle is because the sunken photoeffect that the effect of local light field produces can be widely used in solar cell synergistic technology.2008, the 93rd 073307 phase of volume of periodical Applied Physics Letters once reported that utilizing indium tin oxide surfaces to prepare layer of gold nano particle increased the light trapping effect of solar cell to incident light, made battery efficiency relatively improve 21%.Yet film of metal nano-particles is because the dispersiveness of particle cannot, as independently synergy electrode use, generally adopt tin indium oxide/metal nanoparticle laminated film to use as transparency electrode.And indium in tin indium oxide is a kind of exotic material and has certain toxicity, along with the minimizing of indium resource, certainly will be unfavorable for the sustainable development of photovoltaic industry.
Graphene has hexagonal network structure, has good optical transparence and electroconductibility, can prepare the high-quality Graphene of monoatomic layer or the stack of number atomic shell in existing technology of preparing, and thickness is for number dust is between several nanometers.Utilize these characteristics of Graphene and the surface plasmons effect of metal nanoparticle, develop a kind of Graphene and metal nanoparticle laminated film can address the above problem effectively.
Summary of the invention
technical problem:the object of the invention is to overcome the deficiency of prior art, the preparation method of a kind of Graphene and metal nanoparticle laminated film is provided.In the present invention, Graphene and metal nanoparticle laminated film adopt graphene film, film of metal nano-particles lamination composite structure, utilize the controllability of Graphene thickness to form the surface plasma coupling of (10 nanometers below) of minimum distance between metal nanoparticle, obtain stronger local electric field intensity.And due to the high conductivity of Graphene with thereby optical transparence can be used as the substrate of molecule Raman signal detection or transparent synergy conductive electrode is applied to biological detection and photovoltaic synergy field.
technical scheme:for controlling the coupling distance between nano particle and solving solar cell synergistic transparency electrode problem, the invention provides a kind of method of preparing Graphene and metal nanoparticle laminated film.Technical scheme of the present invention can realize according to following scheme:
Graphene of the present invention and metal nanoparticle laminated film mainly comprise: the first graphene film layer, the second graphene film layer, the 3rd graphene film layer, the first film of metal nano-particles layer and the second film of metal nano-particles layer; This two kinds of thin-film materials of graphene film layer and film of metal nano-particles layer mutually alternately superpose and form Graphene and metal nanoparticle laminated film, and form integral body with base material, as the electrode of solar battery of the substrate of molecule Raman signal detection or transparent synergy.
Described base material adopts silicon chip or silica glass.
The preparation method of a kind of Graphene of the present invention and metal nanoparticle laminated film mainly comprises 5 steps:
A, first utilize chemical Vapor deposition process epitaxy one deck graphene film in copper or nickel metal base, graphene film thickness is for number dust is to tens nanometers, by solution corrosion, fall metal base mode and obtain the first graphene film layer, and be transferred on the surface of base material;
B, using the first graphene film layer and base material integral body as DC electrode, adopt electrophoresis method to put into contain metal nanoparticle solution, at first graphene film layer surface preparation the first film of metal nano-particles layer, or take the first graphene film layer and base material and at the first graphene film layer surface vacuum evaporation layer of metal nano thin-film high temperature annealing, obtain the first film of metal nano-particles layer as whole;
C, in the first film of metal nano-particles, repave and cover the second graphene film layer prepared by one deck chemical Vapor deposition process;
D, the method for utilizing electrophoresis method or vacuum evaporation also to anneal on the second graphene film layer are prepared one deck the second film of metal nano-particles layer;
E, on the second film of metal nano-particles layer, paving is covered the 3rd graphene film layer prepared by one deck chemical Vapor deposition process again.
The first described film of metal nano-particles layer and the single nanoparticle unit pattern of the second film of metal nano-particles layer comprise ball-type, elliposoidal, clavate, set square shape, square, hexagon or disc type, and size is for number nanometer is to tens nanometer.
beneficial effect:the present invention has advantages of following compared with prior art:
1, the preparation method of this Graphene and metal nanoparticle laminated film, to adopt chemical gaseous phase depositing process to prepare Graphene, electrophoresis method or vacuum deposition method are prepared nano particle, therefore can big area prepare this film, have expanded its use and industrialization prospect.
2, the preparation method of this Graphene and metal nanoparticle laminated film, from nano particle preparation process, only need the corresponding metal nanoparticle of preparation nano material can be embedded in laminated film, with this, the size of the gold nano grain being deposited, pattern will can not suffer restraints yet, and settled density can be by regulating different technical parameters to obtain simultaneously.Therefore can prepare the laminated film of different optical character.
3, the preparation method of this Graphene and metal nanoparticle laminated film, utilized the sealing coat effect of the second graphene film layer, can make the first layer and second layer metal nanometer particle film have extremely strong optical coupled effect, make this laminated film there is strong optical enhancement effect.
4, the preparation method of this Graphene and metal nanoparticle laminated film, sees on the whole and has high transparent and high conductivity, and has optics synergy beneficial effect, of many uses, can be used as biological detection substrate and solar cell transparency electrode and uses.
5, the preparation method of this Graphene and metal nanoparticle laminated film has preparation method variation, and film preparation process is simple, preparation time is short, lower film preparation cost, can obtain considerable economic benefit.
Accompanying drawing explanation
Fig. 1 is Graphene and metal nanoparticle complex thin film structure schematic diagram;
Fig. 2 is the Graphene micro-structure diagram of preparing by chemical Vapor deposition process;
Fig. 3 is that electrophoresis method is prepared film of metal nano-particles method schematic diagram;
Fig. 4 is that vacuum deposition method is prepared film of metal nano-particles method schematic diagram.
Fig. 5 is gold nano grain rear film plane microcosmic schematic diagram;
In figure, have; The first graphene film layer 1, the second graphene film layer 3, the 3rd graphene film layer 5, the first film of metal nano-particles layer 2, the second film of metal nano-particles layer 4, base material 6;
Embodiment
A kind of Graphene proposed by the invention and the preparation method of metal nanoparticle laminated film, from step, mainly be divided into graphene film preparation and film of metal nano-particles preparation, but whole laminated film is not the above two functions to be simply added, this Graphene and metal nanoparticle laminated film can show unique optics, electrology characteristic, the surface plasma body resonant vibration that had not only had the high light transmittance of Graphene but also possessed nano particle strengthens characteristic, simultaneously because two layers of nanoparticles is kept apart by Graphene, form the more resonance effect of small distance and greatly strengthened the sunken light of laminated film and the optical property that local strengthens.
In technique preparation, first the technical program is achieved in that, by chemical Vapor deposition process, prepare one deck graphene film, mode by molecule extension generates graphene film on the films such as metal material of copper or nickel, by the mode of liquid corrosion, remove metal again, corrode after metallic film, then the base material that Graphene is transferred to application completes the preparation of the first graphene film layer as silicon chip or silica glass etc.After the first graphene film layer preparation, can adopt following two kinds of modes to prepare the first film of metal nano-particles layer:
I) electrophoretic method is prepared film of metal nano-particles.Using the first graphene layer and base material as DC electrode, and put into another electrode (as metal plate) solution that contains metal nanoparticle simultaneously, utilize the charging property of metal nano material (according to the preparation method of different nanoparticles solution, metal nanoparticle may contain positive charge or negative charge), under the effect of volts DS, metal nanoparticle is deposited on the upper surface of Graphene and substrate laminated film, complete the preparation of the first film of metal nano-particles layer, this method can regulator solution in metal nanoparticle concentration, the parameters such as voltage are controlled the density of metal nanoparticle deposition.
Ii) vacuum deposition method is prepared metal nanoparticle.The first graphene layer and base material as a whole, at its surface vacuum evaporation one deck metal nanometer thin film as thin as a wafer, general thickness is number nanometers or tens nanometers.Then utilize high temperature annealing, metallic film forms film of metal nano-particles under surface tension effects.This method can be controlled thickness of metal film, steps back temperature, annealing time is controlled nano particle size and settled density.
By above-mentioned Graphene method and the film of metal nano-particles method prepared, on base material, prepare again successively the second graphene film layer, the second film of metal nano-particles layer, the 3rd graphene film layer, finally form Graphene of the present invention and metal nanoparticle laminated film.
From embodiment and operating process, mainly the preparation by five layers of nano material completes, below all embodiment under prerequisite, implement take technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
Adopt process for preparing graphenes by chemical vapour deposition and be transferred in quartz substrate
First the 50 micron copper foil levels that clean up are put into vacuum tube furnace, by tube furnace from 30 ° of C through within 70 minutes, being heated to 1000 ° of C.And then pass into the argon gas of 40 milliliters of per minutes and the hydrogen of 40 milliliters of per minutes as protective atmosphere.Under 1000 ° of C, be incubated 30 minutes. the hydrogen of the methane of 10 milliliters of per minutes and 30 milliliters of per minutes is passed in tube furnace, pressure is adjusted to 130 handkerchiefs again.Time is 10 minutes.With 15 ° of C of per minute, drop to room temperature afterwards, complete the growth of graphene film 1.Graphene micro-structure diagram is shown in Fig. 2.After having grown, Graphene spin coating one deck polymethylmethacrylate organic solvent that growth is obtained, is placed on afterwards on the warm table of 120 ° of C and dries 2 minutes. and copper is removed in the ammonium persulfate solution corrosion of putting into again 0.5 mole every liter.Afterwards polymethylmethacrylate/the Graphene wafing on the water surface is picked up with slide glass, put into deionized water rinsing, remove remaining copper ion.And polymethylmethacrylate/Graphene is transferred in quartz substrate 6, with hot acetone, remove polymethylmethacrylate, complete graphene film and quartz substrate laminated film 23.
Embodiment 2:
Utilize electrophoretic method to prepare film of metal nano-particles layer
First in 7.5 ml concns are the cetyl trimethylammonium bromide of 0.1 mole every liter, adding 0.25 ml concn is the golden solution chlorate of 0.01 mole every liter, then to add 0.6 ml concn be that the sodium borohydride solution of 0.01 mole every liter forms gold seeds solution.In beaker, adding successively 38 milliliters of ionized waters, 8 ml concns is that 0.1 mole of every liter of cetyl trimethylammonium bromide, 1 ml concn are that the golden chloric acid of 0.01 mole every liter, the xitix that 3 ml concns are 0.01 mole every liter form growth solution again, again gold seeds solution is got to 10 microlitres and splash in above-mentioned growth solution and stir, growth obtains gold nano grain 21 and solution 22.Using Graphene/quartz substrate laminated film 23 in example 1 as the negative pole of DC electrode, and put into gold nano solution with metal electrode 24, under the effect of direct supply 25, gold nano grain 21 is evenly attached on Graphene and quartz substrate film 23, completes the preparation of the first film of metal nano-particles layer.Fig. 5 is shown in by microscopic appearance schematic diagram.
Embodiment 3
Utilize vacuum deposition method to prepare film of metal nano-particles layer
Adopt vacuum deposition method on graphene film and quartz substrate laminated film 23 surfaces, to prepare the gold nanometer film 26 of one deck 1 to 20 nanometer thickness, by in nitrogen or hydrogen furnace, under 450 ° of C high temperature, anneal and obtain gold nano grain 21 in 30 minutes, complete the preparation of the first film of metal nano-particles layer.
Embodiment 4
Prepare Graphene and metal nanoparticle laminated film
Utilize embodiment 1,2, the methods such as 3 are prepared graphene film 3, film of metal nano-particles 4,5 three layers of nano material of graphene film successively.Finally obtain Graphene and metal nanoparticle laminated film.
The foregoing is only better embodiment of the present invention; protection scope of the present invention is not limited with above-mentioned embodiment; in every case the equivalence that those of ordinary skills do according to disclosed content is modified or is changed, and all should include in the protection domain of recording in claims.
Claims (3)
1. the preparation method of a Graphene and metal nanoparticle laminated film, it is characterized in that, this Graphene and metal nanoparticle laminated film mainly comprise: the first graphene film layer (1), the second graphene film layer (3), the 3rd graphene film layer (5), the first film of metal nano-particles layer (2) and the second film of metal nano-particles layer (4); This two kinds of thin-film materials of graphene film layer and film of metal nano-particles layer mutually alternately superpose and form Graphene and metal nanoparticle laminated film, and form integral body with base material (6), as the electrode of solar battery of the substrate of molecule Raman signal detection or transparent synergy;
This method mainly comprises 5 steps:
A, first utilize chemical Vapor deposition process epitaxy one deck graphene film in copper or nickel metal base, graphene film thickness is for number dust is to tens nanometers, by solution corrosion, fall metal base mode and obtain the first graphene film layer (1), and be transferred on the surface of base material (6);
B, using the first graphene film layer (1) and base material (6) are whole, as DC electrode, adopt electrophoresis method to put into contain metal nanoparticle solution, at first graphene film layer (1) surface preparation the first film of metal nano-particles layer (2), or take the first graphene film layer (1) and base material (6) and at the first graphene film layer (1) surface vacuum evaporation layer of metal nano thin-film high temperature annealing, obtain the first film of metal nano-particles layer (2) for integral body;
C, in the first film of metal nano-particles (2), repave and cover the second graphene film layer (3) prepared by one deck chemical Vapor deposition process;
D, the method for utilizing electrophoresis method or vacuum evaporation also to anneal on the second graphene film layer (3) are prepared one deck the second film of metal nano-particles layer (4);
E, on the second film of metal nano-particles layer (4), paving is covered the 3rd graphene film layer (5) prepared by one deck chemical Vapor deposition process again.
2. the preparation method of a kind of Graphene according to claim 1 and metal nanoparticle laminated film, is characterized in that, described base material (6) adopts silicon chip or silica glass.
3. the preparation method of a kind of Graphene according to claim 1 and metal nanoparticle laminated film, that the single nanoparticle unit pattern that it is characterized in that the first described film of metal nano-particles layer (2) and the second film of metal nano-particles layer (4) comprises is spherical, elliposoidal, clavate, set square shape, square, hexagon or disc type, and size arrives tens nanometer for number nanometers.
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