CN102176382B - Method for preparing grapheme-quantum dot composite film and solar battery structured by using same - Google Patents
Method for preparing grapheme-quantum dot composite film and solar battery structured by using same Download PDFInfo
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- CN102176382B CN102176382B CN2011100367483A CN201110036748A CN102176382B CN 102176382 B CN102176382 B CN 102176382B CN 2011100367483 A CN2011100367483 A CN 2011100367483A CN 201110036748 A CN201110036748 A CN 201110036748A CN 102176382 B CN102176382 B CN 102176382B
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Abstract
The invention relates to a method for preparing a grapheme-quantum dot composite film and a solar battery structured by using the same. The method comprises the following steps of: performing suction filtering on a suspension of grapheme-quantum dot composite powder on a filtering film to obtain a film; and then dissolving the filtering film away with an organic solvent, and transferring the filmto a conductive substrate. The method is characterized in that the ratio of the quantum dot to the grapheme and the thickness of the film can be controlled effectively; in addition, since the film isprepared at normal temperature, the requirement on the conductive substrate is reduced greatly. The prepared film can be used for structuring a novel quantum dot sensitized solar battery. The structured solar battery is of a layer structure, consists of the grapheme-quantum dot film on the conductive substrate, an electrolyte layer and a counter electrode and has the advantages of low cost, simpleness in preparation process, low temperature and stable performance. By the use of the grapheme-quantum dot composite film prepared by the method provided by the invention, the photoelectron transmission performance can be improved, and the photoelectric conversion efficiency of a battery can be enhanced.
Description
Technical field
The present invention relates to the application in a kind of Graphene-quantum dot preparation method of composite film and the constructed quantum dot sensitized solar cell.Belong to area of solar cell
Background technology
Constantly exhausted at the energy, today that environmental consciousness constantly strengthens, the application of solar cell has obtained paying close attention to widely.There is the researcher to propose, narrow gap semiconductor is adsorbed onto on the wide band gap semiconducter surface, overcome the defective of catching sunlight a little less than the wide band gap semiconducter itself, the spectral response of battery is widened visible region, this battery is exactly quantum dot sensitized solar cell (QDSSC).
Typical QDSSC battery is comprised of electrode transparent conducting glass, porous nanometer thin films and quantum dot, electrolyte and platinum.Quantum dot sensitized have a lot of distinctive advantages, such as: by changing the size of particle, can regulate at an easy rate semi-conductive band gap and spectral absorption scope; Light absorption is the band edge type, is conducive to effective collection of sunlight; The surface modification of particle can increase photostability; The natural dipole moment of semiconductor-quantum-point can make electric charge separate fast; Quantum dot absorbs 1 photon can produce a plurality of light induced electrons.So the development of QDSSCs receives the concern of Many researchers all the time.
Quantum dot sensitized process adopts chemical bath (Yu usually, P.R., et al., Journal of PhysicalChemistry B, 2006.110:25451) and electrochemical deposition (Shalom, M., et al., Journal ofPhysical Chemistry C, 2009.113 (9): 3895) etc.The common random dispersion of the quantum dot that obtains in this case is on photoanode surface, the quantity of quantum dot deposition is wayward, it is compound that surface coverage quantum dot lower and undue accumulation easily produces charge carrier, limits density of photocurrent and then affect electricity conversion.
Therefore how establishment quantum point is reunited, and promotes its dispersiveness, and improving simultaneously photoelectronic transmission rate is present quantum dot sensitized solar cell urgent problem.The present invention utilizes the method for suction filtration film forming to prepare the laminated film of Graphene-quantum dot, one side has guaranteed the Uniform Dispersion of quantum dot and then has effectively avoided the probability of electronics and hole-recombination, utilize on the other hand the electric conductivity of Graphene excellence to increase the electric conductivity of film, guaranteed the greatly enhancing of the electricity conversion of corresponding solar cell.
Summary of the invention
The object of the invention is to overcome the shortcoming of prior art, a kind of Graphene-preparation method of quantum dot laminated film and the solar cell of structure are provided.The invention is characterized in that the Graphene that will have excellent electronic transmission performance is incorporated in the quantum dot, replace traditional porous nanometer thin films, and be built into the quantum dot sensitized solar cell of new structure.
Described Graphene-quantum dot laminated film, its preparation method comprises the steps:
(1) be raw material with natural graphite powder, add by a certain percentage sodium nitrate (0.1-5g/ (1g graphite)), the cold concentrated sulfuric acid (10-100ml/ (1g graphite)) and potassium permanganate (0.5-10g/ (1g graphite)), when being lower than 20 ℃, evenly mix, be warming up to subsequently 30-40 ℃ of reaction 25-35min.In above-mentioned mixed solution, slowly add the deionized water dilution, be warming up to 95-100 ℃ of reaction 10-20min, add again a certain amount of hydrogenperoxide steam generator (5-50ml/ (1g graphite)); Then with mentioned solution centrifugal filtration, and remove metal ion with dilute hydrochloric acid solution washing, remove unnecessary acid with the deionized water washing again, and repeatedly be washed with water to neutrality, finally obtain the oxidized graphite flake aqueous solution, again it is carried out ultrasonic processing, obtain the graphene oxide solution that filemot homogeneous disperses.
(2) get the graphene oxide solution that above-mentioned homogeneous disperses, add quantum dot particle or quantum dot reaction precursor liquid formation graphene oxide-quantum dot mixed liquor by 1: 1～1: 50 mass ratio.
(3) in above-mentioned graphene oxide-quantum dot mixed solution, add the reducing agent hydrazine hydrate, stir 24h at 80 ℃, after reduction reaction, resulting product is carried out ultrasonic processing, then centrifugal removal precipitates on a small quantity, and the centrifugal stable suspension that obtains is Graphene-quantum dot solution.
(4) Graphene in above-mentioned (3)-quantum dot solution is diluted, stirs until form uniform and stable suspension.
(5) with above-mentioned Graphene-quantum dot suspension vacuum filtration, form film at untreated filter membrane.
(6) or use the filter membrane processed, its technical process is: with the suspension vacuum filtration of oxide particle, deposit one deck sull at untreated filter membrane.And then suction filtration Graphene-quantum dot suspension is deposited on the filter membrane of processing.
(7) film that closely is connected on the filter membrane that after the massive laundering step (5) is formed is fixed on the base material.
(8) then put into baking oven 55-65 ℃ of vacuumize 6h-24h, with acetone filter membrane is dissolved subsequently, obtain the film of Graphene-quantum dot on conductive substrates.
(9) film that closely is connected on the filter membrane that after the massive laundering step (6) is formed is fixed on the base material, can obtain subsequently the film of Graphene-quantum dot on conductive substrates of composite oxide film according to step (8).
Described quantum dot particle is CdSe, CdS, CdTe, InP, PbS, InN, Ta
3N
5, GaAs, GaP, ZnO, Fe
2O
2, WO
3, SnO
2And TiO
2In one or more particles.
Described quantum dot reaction precursor liquid is Cd (NO
3)
2, CdCl
2, Pb (NO
3)
2, PbCl
2, K
2S, Na
2S, H
2S, NaSeSO
3, TiCl
4, NH
4In OH, HCl and phthalandione four butyl esters one or more, purpose is that original position generates Graphene-quantum dot solution.
Described sull is TiO
2, ZnO, ZnS, SnO
2, Nb
2O
5, Al
2O
3, In
2O
3, CuO and SiO
2In one or more sulls.
Described base material is transparent conducting glass, metallic substrates, material with carbon element substrate or polyethylene, polystyrene and polyester macromolecule substrate.
The Graphene of described preparation-quantum dot laminated film can be configured to quantum dot sensitized solar cell.Constructed solar cell is layer structure, and namely the Graphene on the conductive substrates-quantum dot laminated film in laminated film By Electrolysis matter, then covers upper to electrode.
Described electrolyte is acetonitrile, valeronitrile, methoxypropionitrile, ethylene carbonate, propene carbonate, gamma-butyrolacton, elemental iodine, lithium iodide, the liquid electrolyte of one or more in pyridinium iodide and the fuse salt, it perhaps is glucitol derivative, the copolymer of vinylidene and hexafluoropropylene, acrylic acid polymer, trimethoxy silane, many pyridines side chain type polyamide dendroid macromolecular derivatives, the quasi-solid electrolyte of one or more in Nano particles of silicon dioxide and the carbon nano-particle perhaps is cuprous rhodanide, cuprous iodide, NiO, poly-(3-octyl group thiophene), polypyrrole, polyoxyethylene, polyacrylonitrile, the copolymer of epoxychloropropane and oxirane and one or more the solid electrolyte in the Kynoar.
Described is a kind of in metal electrode, material with carbon element electrode and the macromolecule electrode to electrode.
Advantage by the Graphene of the present invention preparation-quantum dot laminated film is: the quantity that can effectively control quantum dot in the film, while Graphene Uniform Dispersion in film, made up good conductive network, can provide fast passage for photoelectronic transmission at the quantum dot sensitized solar cell that is built into by prepared laminated film, reduced the probability of photoelectron and hole-recombination, this transmits it to external circuit so that conductive substrates can be collected photoelectron effectively, thereby improves the electricity conversion of battery.(seeing embodiment for details)
Description of drawings
Fig. 1 is that gained ratio of the present invention is the transmission electron microscope photo (TEM) of 1: 1.5 Graphene-Quantum dots CdS e;
Fig. 2 is that gained ratio of the present invention is the transmission electron microscope photo (TEM) of 1: 9 Graphene-Quantum dots CdS e;
Fig. 3 is by the Graphene of the present invention's preparation-constructed quantum dot sensitized solar battery structure figure of quantum dot laminated film.Wherein 1, to electrode; 2, electrolyte, 3, sull; 4, Graphene-quantum dot film; 5, conductive substrates.
Embodiment
The present invention will be described in detail below in conjunction with embodiment, but the present invention is not limited to following examples.
Embodiment 1: the preparation method of a kind of Graphene-quantum dot laminated film comprises the steps:
(1) is raw material with the 1g natural graphite powder, adds 0.8g sodium nitrate, the cold concentrated sulfuric acid and 3g potassium permanganate, when being lower than 20 ℃, evenly mix, be warming up to subsequently 35 ℃ of reaction 30min.In above-mentioned mixed solution, slowly add the deionized water dilution, be warming up to 98 ℃ of reaction 15min, add again 30% hydrogenperoxide steam generator of 10ml; Then with mentioned solution centrifugal filtration, and remove metal ion with dilute hydrochloric acid solution washing, remove unnecessary acid with the deionized water washing again, and repeatedly be washed with water to neutrality, finally obtain the oxidized graphite flake aqueous solution, again it is carried out ultrasonic processing, obtain the graphene oxide solution that filemot homogeneous disperses.
(2) get the graphene oxide solution that above-mentioned homogeneous disperses, add Cd (NO3) 2 and NaSeSO3 and NH in 1: 4.5 ratio
4OH, reaction generates graphene oxide-Quantum dots CdS e solution.
(3) in above-mentioned graphene oxide-quantum dot solution, add the reducing agent hydrazine hydrate, stir 24h at 80 ℃, after reduction reaction, resulting product is carried out ultrasonic processing, then centrifugal removal precipitates on a small quantity, and the centrifugal stable suspension that obtains is Graphene-Quantum dots CdS e solution.
(4) with above-mentioned Graphene-Quantum dots CdS e solution dilution, stirring until form uniform and stable suspension.
(5) first at filter membrane deposition one deck TiO
2Film.Then suction filtration Graphene-Quantum dots CdS e suspension is deposited on this filter membrane.
The film that (6) will closely be connected on the filter membrane after the massive laundering is fixed on the base material, and sample is put into 60 ℃ of vacuumize 12h of baking oven, with acetone filter membrane is dissolved subsequently, obtains composite Ti O
2Graphene-the quantum dot film of film.
Embodiment 2: the preparation process in the present embodiment and step and above-described embodiment 1 are identical.Different is: graphene oxide mixes according to 1: 1.5 ratio with reactant liquor. and Fig. 1 is transmission electron microscope (TEM) the photo figure of this embodiment.
Embodiment 3: the preparation process in the present embodiment and step and above-described embodiment 1 are identical.Different is: graphene oxide mixes according to 1: 6 ratio with reactant liquor.
Embodiment 4: the preparation process in the present embodiment and step and above-described embodiment 1 are identical.Different is: graphene oxide mixes according to 1: 9 ratio with reactant liquor. and Fig. 2 is transmission electron microscope (TEM) the photo figure of this embodiment.
Composite Ti O with above-described embodiment 1,2,3 and 4 preparations
2Graphene-the quantum dot film of film makes up quantum dot sensitized solar cell.Constructed solar cell is layer structure, i.e. composite Ti O on the electro-conductive glass
2Graphene-the quantum dot film of sull is liquid electrolyte acetonitrile, elemental iodine and lithium iodide at laminated film, then covers upper platinum to electrode.Fig. 3 is the quantum dot sensitized solar battery structure figure that the present embodiment makes up, wherein TiO
2The thickness of sull is 400nm, and the thickness of Graphene-quantum dot film is 7 μ m.
Comparative example 1: any is identical among the preparation process in the present embodiment and step and above-described embodiment 1-4.Unique different be as a comparison, employed Graphene-quantum dot film is to use traditional chemical bath method that base material is impregnated in Graphene-quantum dot solution, then obtains after the oven dry.
Table 1 is the photoelectric properties index of having listed the quantum dot sensitized solar cell of embodiment 1-4 and comparative example 1 preparation.
Table 1
As shown in Table 1, use the photoelectric conversion efficiency of the Graphene of preparation method provided by the invention preparation-solar cell that quantum dot laminated film (embodiment 1-4) makes up between 0.30-0.80%, far above the conversion efficiency of comparative example 1.
Claims (10)
1. Graphene-quantum dot laminated film is characterized in that the preparation method comprises the steps:
(1) be raw material with natural graphite powder, add a certain amount of sodium nitrate, the cold concentrated sulfuric acid and potassium permanganate, when being lower than 20 ℃, evenly be mixed to get mixed solution, be warming up to subsequently 30-40 ℃ of reaction 25-35min, in above-mentioned mixed solution, slowly add the deionized water dilution, be warming up to 95-100 ℃ of reaction 10-20min, add again a certain amount of hydrogenperoxide steam generator; The solution centrifugal that then will add hydrogen peroxide filters, and remove metal ion with dilute hydrochloric acid solution washing, remove unnecessary acid with the deionized water washing again, and repeatedly be washed with water to neutrality, finally obtain the oxidized graphite flake aqueous solution, again it is carried out ultrasonic processing, obtain the graphene oxide solution that filemot homogeneous disperses; By every 1g graphite powder, the sodium nitrate amount that adds respectively is 0.1-5g, and the concentrated sulfuric acid amount of adding is 10-100ml, and the potassium permanganate amount of adding is 0.5-10g, and the hydrogenperoxide steam generator amount of adding is 5-50ml;
(2) get the graphene oxide solution that the homogeneous of above-mentioned steps (1) disperses, by 1: 1-1: 50 mass ratioes add the quantum dot particle or quantum dot reaction precursor liquid forms graphene oxide-quantum dot mixed liquor;
(3) in the graphene oxide of above-mentioned steps (2)-quantum dot mixed solution, add the reducing agent hydrazine hydrate, stir 24h at 80 ℃, after reduction reaction, resulting product is carried out ultrasonic processing, then centrifugal removal precipitates on a small quantity, and the centrifugal stable suspension that obtains is Graphene-quantum dot solution;
(4) with the Graphene of above-mentioned steps (3)-quantum dot solution dilution, stir until form uniform and stable suspension;
(5) with the Graphene of above-mentioned steps (4)-quantum dot suspension vacuum filtration, form film at untreated filter membrane; Above-mentioned steps (5) or be that (5) use the filter membrane processed, its treatment process is: with the suspension vacuum filtration of oxide particle, deposit one deck sull at untreated filter membrane; And then suction filtration Graphene-quantum dot suspension is deposited on the filter membrane of processing;
(6) after the massive laundering film that closely is connected on the filter membrane in (5) is fixed on the base material;
(7) then put into baking oven 55-65 ℃ of vacuumize 6h-24h, with acetone filter membrane is dissolved subsequently, obtain the film of Graphene-quantum dot on conductive substrates.
2. laminated film according to claim 1 is characterized in that described quantum dot particle is CdSe, CdS, CdTe, InP, PbS, InN, Ta
3N
5, GaAs, GaP, ZnO, Fe
2O
2, WO
3, SnO
2And TiO
2In one or more particles.
3. laminated film according to claim 1 is characterized in that described quantum dot reaction precursor liquid is Cd (NO
3)
2, CdCl
2, Pb (NO
3)
2, PbCl
2, K
2S, Na
2S, H
2S, NaSeSO
3, TiCl
4, NH
4In OH, HCl and phthalandione four butyl esters one or more, original position generates Graphene-quantum dot solution.
4. laminated film according to claim 1 is characterized in that described sull is TiO2, ZnO, ZnS, SnO
2, Nb
2O
5, Al
2O
3, In
2O
3, CuO and SiO
2In one or more sulls.
5. laminated film according to claim 1, it is characterized in that described base material be transparent conducting glass, metallic substrates, material with carbon element substrate, polyvinyl at the bottom of, polystyrene substrate or polyester base.
6. the solar cell that is made up by the Graphene of each preparation among the claim 1-5-quantum dot laminated film, it is characterized in that constructed solar cell is layer structure, namely by the Graphene on the conductive substrates-quantum dot laminated film, electrolyte on laminated film and electrolyte cover electrode is consisted of.
7. solar cell according to claim 6 is characterized in that described electrolyte is liquid electrolyte, quasi-solid electrolyte or solid electrolyte.
8. solar cell according to claim 7, it is characterized in that described electrolyte is acetonitrile, valeronitrile, methoxypropionitrile, ethylene carbonate, propene carbonate, gamma-butyrolacton, elemental iodine, lithium iodide, the liquid electrolyte of one or more in pyridinium iodide and the fuse salt, it perhaps is glucitol derivative, the copolymer of vinylidene and hexafluoropropylene, acrylic acid polymer, trimethoxy silane, many pyridines side chain type polyamide dendroid macromolecular derivatives, the quasi-solid electrolyte of one or more in Nano particles of silicon dioxide and the carbon nano-particle perhaps is cuprous rhodanide, cuprous iodide, NiO, poly-(3-octyl group thiophene), polypyrrole, polyoxyethylene, polyacrylonitrile, the copolymer of epoxychloropropane and oxirane and one or more the solid electrolyte in the Kynoar.
9. solar cell according to claim 6 is characterized in that described is a kind of in metal electrode, material with carbon element electrode and the macromolecule electrode to electrode.
10. solar cell according to claim 6, the photoelectric conversion efficiency that it is characterized in that constructed solar cell is between the 0.30-0.80%.
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