CN102660740A - 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 the nano material preparation technical field, specifically is the preparation method of a kind of Graphene and metal nanoparticle laminated film.
Background technology
In recent years; Graphene and metal nanoparticle have great application prospect because its unique optics, electricity, mechanics and characteristics such as katalysis and physiologically acceptable have caused extensive interest in the nanosecond science and technology field in electron transport device, electrode capactitance device, transmitter, Single Molecule Detection, photovoltaic synergy and prepare composite.
The special property of metal nanoparticle such as surface plasma excimer effect are because the nano grain surface unbound electron receives electric field component excitation in the incident electromagnetic wave (or incident light), interact and produce, and form surface plasma excimer.This surface plasmon can produce an increase higher than the incident electromagnetic wave (or incident)
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times the local electric field strength.Because the high strength of electric field of local is of value to the amplification of unit molecule raman detection signal and improves solar device to the absorption of incident light rate, and is once becoming the hot technology in biomolecule detection and the photovoltaic synergy field.In field of biological detection; Discover; When metal nanoparticle is coupled near generation each other, can changes 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 (below 10 nanometers) is comparatively difficult at the nano material preparation technical elements, generally can only accomplish the above distance of 10 nanometers through traditional nanoimprinting technology, 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 owing to the sunken photoeffect that the effect of local light field produces can be widely used in the solar cell synergistic technology.2008, the 93rd 073307 phase of volume of periodical Applied Physics Letters reported once that utilizing indium tin oxide surfaces to prepare one deck gold nano grain increased the sunken light action of solar cell to incident light, made battery efficiency improve 21% relatively.Yet film of metal nano-particles is because the particulate dispersiveness can't generally adopt tin indium oxide/metal nanoparticle laminated film to use as transparency electrode as independently synergy electrode use.And the indium in the 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 the hexagonal network structure, has good optical transparence and electroconductibility, technical monoatomic layer or the synergetic high-quality Graphene of number atomic shell prepared of existing preparation, and thickness arrives between several nanometers for the number dust.Utilize these characteristics of Graphene and the surface plasmons effect of metal nanoparticle, develop a kind of Graphene and the metal nanoparticle laminated film can address the above problem effectively.
Summary of the invention
Technical problem:The objective 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.Graphene and metal nanoparticle laminated film adopt graphene film, film of metal nano-particles lamination composite structure among the present invention; Utilize the controllability of Graphene thickness to form the surface plasma coupling of minimum distance between the metal nanoparticle (below 10 nanometers), obtain stronger local electric field intensity.And because the high conductivity of Graphene and 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 coupling distance between the control nano particle and solution solar cell synergistic transparency electrode problem, the invention provides a kind of method for 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 alternately superpose each other and form Graphene and metal nanoparticle laminated film; And whole with the base material formation, as substrate of molecule raman signal detection or transparent synergic electrode of solar battery.
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, at first utilize chemical Vapor deposition process epitaxy one deck graphene film on copper or nickel metal base; Graphene film thickness is for counting dust to tens nanometers; Fall the metal base mode through solution corrosion and obtain the first graphene film layer, and be transferred on the surface of base material;
B, adopt the first graphene film layer and base material integral body electrophoresis method to put into as DC electrode to contain metal nanoparticle solution; Prepare the first film of metal nano-particles layer at the first graphene film laminar surface, or serve as whole to obtain the first film of metal nano-particles layer at the first graphene film laminar surface vacuum evaporation layer of metal nano thin-film and high temperature annealing with the first graphene film layer and base material;
C, on first film of metal nano-particles, repave the second graphene film layer that covers one deck chemical Vapor deposition process preparation;
D, on the second graphene film layer, utilize electrophoresis method or vacuum evaporation and annealed method to prepare one deck second film of metal nano-particles layer;
E, the 3rd graphene film layer of one deck chemical Vapor deposition process preparation is covered in the shop once more on the second film of metal nano-particles layer.
The single nanoparticle unit pattern of the described first film of metal nano-particles layer and the second film of metal nano-particles layer comprises ball-type, elliposoidal, clavate, set square shape, square, hexagon or video disc shape, and size arrives tens nanometer for the number nanometer.
Beneficial effect:The present invention has following advantage compared with prior art:
1, the preparation method of this Graphene and metal nanoparticle laminated film; Be to adopt chemical gaseous phase depositing process to prepare Graphene; Electrophoresis method or vacuum deposition method prepare nano particle, therefore can this film of large-area preparation, enlarged its use and industrialization prospect.
2, the preparation method of this Graphene and metal nanoparticle laminated film; From the preparation of nanoparticles process; Only need preparation corresponding metal nano particle to embed nano material in the laminated film; With this, the size of the gold nano grain that is deposited, pattern will can not suffer restraints yet, and settled density can obtain through regulating different technical parameters 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 that extremely strong optical coupled effect is arranged, make this laminated film have intensive optics enhancement.
4, the preparation method of this Graphene and metal nanoparticle laminated film sees to have high transparent and high conductivity on the whole, and has optics synergy beneficial effect, and is 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 the preparation method variation, and the film preparation process is simple, preparation time short, lower the film preparation cost, can obtain considerable economic.
Description of drawings
Fig. 1 is Graphene and metal nanoparticle complex thin film structure synoptic diagram;
Fig. 2 is the Graphene micro-structure diagram through the chemical Vapor deposition process preparation;
Fig. 3 is that electrophoresis method prepares film of metal nano-particles method synoptic diagram;
Fig. 4 is that vacuum deposition method prepares film of metal nano-particles method synoptic diagram.
Fig. 5 is a gold nano grain rear film plane microcosmic synoptic diagram;
Have among the figure; 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; See 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 function simple addition, and this Graphene and metal nanoparticle laminated film can show unique optics, electrology characteristic, has not only had the high light transmittance of Graphene but also has possessed the surface plasma body resonant vibration enhanced characteristic of nano particle; Simultaneously, form sunken light and local enhanced optical performance that the resonance effect of small distance has more greatly strengthened laminated film because two layers of nanoparticles is kept apart by Graphene.
On prepared; The present technique scheme is achieved in that at first; Prepare one deck graphene film through chemical Vapor deposition process, the mode through the molecule extension generates graphene film on films such as metal material of copper or nickel, remove metal through the mode of liquid corrosion again; After corroding mf, be transferred to the base material of application such as the preparation that silicon chip or silica glass etc. are accomplished the first graphene film layer to Graphene again.After the preparation of the first graphene film layer finishes, can adopt the following prepared in one of two ways first film of metal nano-particles layer:
I) electrophoretic method prepares film of metal nano-particles.First graphene layer and base material as DC electrode; And put into the solution that contains metal nanoparticle simultaneously with another electrode (like metal plate); The charging property of utilizing metal nano material is (according to the preparation method of different nanoparticles solution; Metal nanoparticle possibly 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; Accomplish the preparation of the first film of metal nano-particles layer, this method can regulator solution in the sedimentary density of parameter control metal nanoparticle such as metal nanoparticle concentration, voltage.
Ii) vacuum deposition method prepares metal nanoparticle.First graphene layer and base material as a whole, at its surface vacuum vapor deposition one deck metal nanometer thin film as thin as a wafer, general thickness is number nanometers or tens nanometers.Utilize high temperature annealing then, mf 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 preparation Graphene method and film of metal nano-particles method; The refabrication second graphene film layer, the second film of metal nano-particles layer, the 3rd graphene film layer on base material finally form Graphene of the present invention and metal nanoparticle laminated film successively.
From embodiment and operating process, mainly the preparation through five layers of nano material is accomplished, below all embodiment all be to be to implement under the prerequisite with technical scheme of the present invention, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
The employing process for preparing graphenes by chemical vapour deposition also is transferred on the quartz substrate
The 50 micron copper foil levels that at first will clean up are put into vacuum tube furnace, with tube furnace from 30 ° of C through being heated to 1000 ° of C in 70 minutes.And then the hydrogen of argon gas and 40 milliliters of PMs that feeds 40 milliliters of PMs is as protective atmosphere.Insulation is 30 minutes under 1000 ° of C. and the methane of 10 milliliters of PMs and the hydrogen of 30 milliliters of PMs are fed in the tube furnace, pressure is adjusted to 130 handkerchiefs again.Time is 10 minutes.Drop to room temperature with 15 ° of C of PM afterwards, accomplish the growth of graphene film 1.The Graphene micro-structure diagram is seen Fig. 2.After growth is accomplished,, be placed on the warm table of 120 ° of C oven dry afterwards 2 minutes with Graphene spin coating one deck polymethylmethacrylate organic solvent that growth obtains. put into 0.5 mole every liter ammonium persulfate solution corrosion removing copper again.Polymethylmethacrylate/the Graphene that will waft on the water surface afterwards picks up with slide glass, puts into the deionized water rinsing, removes the remaining copper ion.And polymethylmethacrylate/Graphene transferred on the quartz substrate 6, remove polymethylmethacrylate with hot acetone, accomplish graphene film and quartz substrate laminated film 23.
Embodiment 2:
Utilize electrophoretic method to prepare the film of metal nano-particles layer
Be that to add 0.25 ml concn in 0.1 mole every liter the cetyl trimethylammonium bromide be 0.01 mole every liter golden solution chlorate at 7.5 ml concns at first, the sodium borohydride solution that adds 0.6 ml concn again and be 0.01 mole every liter forms gold seeds solution.In beaker, adding 38 milliliters of ionized waters, 8 ml concns more successively is that 0.1 mole of every liter of cetyl trimethylammonium bromide, 1 ml concn are that 0.01 mole every liter golden chloric acid, the xitix that 3 ml concns are 0.01 mole every liter form growth solution; Get 10 microlitres to gold seeds solution again and splash in the above-mentioned growth solution and stirring, growth obtains gold nano grain 21 and solution 22.The negative pole of Graphene in the instance 1/quartz substrate laminated film 23 as DC electrode; And put into gold nano solution with metal electrode 24; Under the effect of direct supply 25; Gold nano grain 21 evenly attached on Graphene and the quartz substrate film 23, is accomplished the preparation of the first film of metal nano-particles layer.The microscopic appearance synoptic diagram is seen Fig. 5.
Embodiment 3
Utilize vacuum deposition method to prepare the film of metal nano-particles layer
Adopt the gold nano film 26 of vacuum deposition method in graphene film and quartz substrate laminated film 23 surface preparation one decks 1 to 20 nanometer thickness; Through in nitrogen or hydrogen furnace; 450 ° of C high temperature are annealed down and were obtained gold nano grain 21 in 30 minutes, accomplish the preparation of the first film of metal nano-particles layer.
Embodiment 4
Preparation Graphene and metal nanoparticle laminated film
Utilize embodiment 1,2, methods such as 3 prepare 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 above is merely preferred embodiments of the present invention; Protection scope of the present invention is not exceeded with above-mentioned embodiment; As long as the equivalence that those of ordinary skills do according to disclosed content is modified or changed, all should include in the protection domain of putting down in writing in claims.
Claims (4)
1. the preparation method of 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 alternately superpose each other and form Graphene and metal nanoparticle laminated film; And whole with base material (6) formation, as substrate of molecule raman signal detection or transparent synergic electrode of solar battery.
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 is characterized in that, this method mainly comprises 5 steps:
A, at first utilize chemical Vapor deposition process epitaxy one deck graphene film on copper or nickel metal base; Graphene film thickness is for counting dust to tens nanometers; Fall the metal base mode through solution corrosion and obtain the first graphene film layer (1), and be transferred on the surface of base material (6);
B, adopt electrophoresis method to put into as DC electrode to contain metal nanoparticle solution the first graphene film layer (1) and base material (6) are whole; At first graphene film layer (1) surface preparation, the first film of metal nano-particles layer (2), or serve as whole to obtain the first film of metal nano-particles layer (2) at first graphene film layer (1) the surface vacuum vapor deposition layer of metal nano thin-film and high temperature annealing with the first graphene film layer (1) and base material (6);
C, on first film of metal nano-particles (2), repave the second graphene film layer (3) that covers one deck chemical Vapor deposition process preparation;
D, on the second graphene film layer (3), utilize electrophoresis method or vacuum evaporation and annealed method to prepare one deck second film of metal nano-particles layer (4);
E, the 3rd graphene film layer (5) of one deck chemical Vapor deposition process preparation is covered in the shop once more on the second film of metal nano-particles layer (4).
4. the preparation method of a kind of Graphene according to claim 3 and metal nanoparticle laminated film; The single nanoparticle unit pattern that it is characterized in that the described first film of metal nano-particles layer (2) and the second film of metal nano-particles layer (4) comprises ball-type, elliposoidal, clavate, set square shape, square, hexagon or video disc shape, and size arrives tens nanometer for the number nanometer.
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