CN103617891B - A kind of indium tin oxide nanowire array composite and preparation method thereof and application in solar cells - Google Patents
A kind of indium tin oxide nanowire array composite and preparation method thereof and application in solar cells Download PDFInfo
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- CN103617891B CN103617891B CN201310613182.5A CN201310613182A CN103617891B CN 103617891 B CN103617891 B CN 103617891B CN 201310613182 A CN201310613182 A CN 201310613182A CN 103617891 B CN103617891 B CN 103617891B
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Abstract
The invention discloses a kind of indium tin oxide nanowire array composite and preparation method thereof and application in solar cells.Indium tin oxide nanowire array composite, it comprises the tin indium oxide nano-wire array of growth in conductive substrates, and described tin indium oxide nano-wire array is enclosed with cuprous sulfide nano particle.Preparation method provided by the invention comprises the steps: that (1) is catalyst with gold nano grain, by chemical vapour deposition technique, and tin indium oxide nano-wire array described in deposition growing in described conductive substrates; (2) by chemical bath deposition method, coated CdS nano particle on described tin indium oxide nano-wire array; (3) by ion-exchange, described CdS nanoparticle conversion is become Cu
2s nano particle; Then under an inert atmosphere, through calcining and obtain described composite material.Use Cu prepared by the present invention
2sITO nano-wire array is obviously better than precious metals pt or Au as performance after the solar cell formed electrode material, and the transient metal chalcogenide compound of Metal Substrate is as the solar cell to electrode material.
Description
Technical field
The present invention relates to a kind of indium tin oxide nanowire array composite and preparation method thereof and application in solar cells.
Background technology
Along with the fast development of contemporary mankind society, day by day serious energy and environment problem accelerates the development and utilization of new energy technology, solar energy relies on its resource reserve to enrich, the advantages such as clean environment firendly receive the extensive concern of people, and become the focus of research as the solar cell of electrooptical device.Quantum dot sensitized solar cell is as a kind of novel photoelectric switching device, while structurally having used for reference DSSC, organic dye molecule is replaced as light absorbent using inorganic semiconductor quantum dot, not only significantly can reduce production cost, rely on quantum size effect and the multi-electron excitation effect of inorganic-quantum-dot simultaneously, make its theoretical light photoelectric transformation efficiency bring up to 44% from 31%, become the solar cell types that a class has Commercial Prospect very much.But, what be generally used for quantum dot sensitized solar cell at present is precious metals pt or Au catalyst to electrode material, the use of noble metal catalyst not only significantly increases the one-tenth product cost of quantum dot sensitized solar cell, and the ability of its catalytic many sulphur electrolyte generation reduction reaction is also undesirable.Therefore, another kind of based on non-noble metal focus electrode catalyst agent material being become to people's concern.The develop rapidly of nanometer technology since the nineties in 20th century, for the novel preparation of base metal base to electrode catalyst provides new direction.
The more base metal of current research, to an electrode catalyst mainly class transient metal chalcogenide compound, comprises Cu
2s, PbS, CoS, NiS and quaternary compound Cu
2znSnS
4, Cu
2znSnSe
4deng.Because such is stronger for the ability of catalysis many sulphur electrolyte generation reduction reaction to electrode catalyst, thus show catalytic performance more better than noble metal catalyst.But, due to the attribute of the semiconductor of these this kind of materials itself, in the process of preparation or based on corresponding metallic substrates, the such as conventional Cu based on brass substrate
2s, or need the nano particle obtained and other conductive additives such as carbon black or Graphene to carry out compound.Owing to there is metallic substrates in the former, meeting and many sulphur electrolyte slowly react, thus affect the stability of battery; The latter not only needs Kaolinite Preparation of Catalyst material and conductive additive respectively, and the factor such as the character of electric conducting material itself and the uniformity of compound directly can restrict the catalytic performance to electrode, and newly add material and may introduce new interface to electrode, thus increase the series resistance of battery.Therefore, how to improve the catalytic performance of electrode material and then obtain efficient quantum dot sensitized solar cell and still there is very large challenge.
Therefore, provide a kind of simple, low cost to electrode material and technology of preparing thereof, and efficiently, to be stably of great significance for quantum dot sensitized solar cell tool.
Summary of the invention
The object of this invention is to provide a kind of indium tin oxide nanowire array composite and preparation method thereof and application in solar cells.
A kind of indium tin oxide nanowire array composite (Cu provided by the present invention
2sITO), it comprises the tin indium oxide nano-wire array of growth in conductive substrates, and described tin indium oxide nano-wire array is enclosed with cuprous sulfide nano particle.
In above-mentioned composite material, in described tin indium oxide nano-wire array, the length of tin indium oxide nano-wire can be 1 micron ~ 30 microns, specifically can be 3 microns ~ 10 microns, 3 microns, 7 microns or 10 microns, diameter can be 50 nanometer ~ 300 nanometers, specifically can be 100 nanometer ~ 120 nanometers, 100 nanometers, 110 nanometers or 120 nanometers.
In above-mentioned composite material, the particle diameter of described cuprous sulfide nano particle can be 5 nanometer ~ 100 nanometers, specifically can be 15 nanometer ~ 30 nanometers;
The thickness of the layer structure that described cuprous sulfide nano particle is formed can be 10 ~ 50 nanometers, as 20 nanometers.
Described conductive substrates can be indium oxide tin glass (ITO) or fluorine-doped tin oxide glass (FTO) etc.
The present invention still further provides the preparation method of described composite material, comprises the steps:
(1) be catalyst with gold nano grain, by chemical vapour deposition technique, tin indium oxide nano-wire array described in deposition growing in described conductive substrates;
(2) by chemical bath deposition method, coated CdS nano particle on described tin indium oxide nano-wire array;
(3) by ion-exchange, described CdS nanoparticle conversion is become Cu
2s nano particle; Then under an inert atmosphere, through calcining and obtain described composite material.
In above-mentioned preparation method, in step (1), the particle diameter of described gold nano grain can be 2 ~ 10 nanometers, specifically can be 5 nanometers;
The indium source growing described tin indium oxide nano-wire array used can be indium metal and/or indium oxide;
The Xi Yuan growing described tin indium oxide nano-wire array used can be metallic tin and/or tin oxide;
The mol ratio of described indium source and described Xi Yuan can be 1 ~ 30:1, specifically can be 10:1.
In above-mentioned preparation method, in step (1), indium source used for the described tin indium oxide nano-wire array of growth and Xi Yuan are heated into gaseous state, as heated at 800 DEG C under the condition of 600 ~ 1000 DEG C;
The growth course of described tin indium oxide nano-wire array is carried out in crystallizing field, and the temperature of described crystallizing field can be 300 ~ 550 DEG C, and growth time can be 5 ~ 120 minutes, as grown 20 minutes under the condition of 400 DEG C.
In above-mentioned preparation method, in step (2), the cadmium salt that described chemical bath deposition method uses can be at least one in cadmium acetate, caddy, cadmium sulfate and cadmium nitrate;
The sulfosalt that described chemical bath deposition method uses can be at least one in sulphur powder, thiocarbamide, thiosemicarbazides and thioacetamide;
The temperature of described chemical bath deposition method can be 0 ~ 80 DEG C, and the time can be 0.1 ~ 8 hour, specifically can deposit 2 hours under the condition of 25 DEG C.
In above-mentioned preparation method, in step (3), described ion-exchange comprises the steps:
The tin indium oxide nano-wire array of coated CdS nano particle step (2) obtained is transferred in the aqueous solution of mantoquita, through ion-exchange reactions, becomes Cu by described CdS nanoparticle conversion
2s nano particle;
Described mantoquita is at least one in cuprous acetate, stannous chloride and cuprous sulfate;
The temperature of described ion-exchange reactions can be 5 ~ 90 DEG C, and the time can be 0.5 ~ 60 minute, specifically can exchange 5 minutes under the condition of 50 DEG C.
In above-mentioned preparation method, in step (3), the temperature of described calcining can be 250 ~ 500 DEG C, and the time can be 10 ~ 60 minutes, specifically can calcine 30 minutes under the condition of 400 DEG C.
Indium tin oxide nanowire array composite prepared by the present invention can be used as solar cell to electrode, described solar cell can be quantum dot sensitized solar cell or DSSC etc.In described indium tin oxide nanowire array composite, tin indium oxide nano-wire array wherein and conductive substrates form three-dimensional conductive network, what the electronics collected electrode can be exceedingly fast is injected in electrode catalyst, then utilizes the Cu with high-efficiency catalytic activity of load on conductive network
2s catalyst carries out the reduction reaction of effective catalytic electrolysis matter, therefore uses composite material of the present invention as to electrode, has that method is simple, cost is low, catalytic activity is high and the plurality of advantages such as long-term stability.
Compare with other prior aries, the present invention has following characteristics:
1, the tin indium oxide nano-wire array adopting chemical vapour deposition technique to prepare in the present invention, the structure due to its monocrystalline makes electronics can transmit fast in nano wire and can not be subject to the inhibition of crystal boundary; Simultaneously because tin indium oxide nano-wire array provides three-dimensional catalyst carrier, the load capacity that greatly can improve catalyst and then the catalytic efficiency improved electrode.
2, the present invention adopts Cu
2s nano particle to electrode catalyst as highly active, owing to adopting the tin indium oxide nano-wire array of conduction to instead of traditional metallic substrates, as copper, make describedly electrode is not existed to the problem of slowly being corroded by many sulphur electrolyte, thus has better stability.
3, the Cu prepared by the inventive method
2sITO nano-wire array, owing to passing through chemical bath deposition and ion-exchange process in-situ preparation Cu
2s, the interface between itself and ITO is very good.Wherein Cu
2sITO nano-wire array utilizes heavily doped P type semiconductor to contact with heavily doped N type semiconductor, can form good ohmic contact, is conducive to the injection of electronics; Be injected into Cu
2after S, due to this layer of Cu
2s thickness is in tens nanometers, and electronics is easy to through Cu
2s and arrive electrolyte interface, thus substantially reduce battery operated in series resistance, the remarkable solar energy conversion efficiency improving battery.
4, the Cu using the present invention to prepare
2sITO nano-wire array is obviously better than precious metals pt or Au as performance after the solar cell formed electrode material, and the transient metal chalcogenide compound of Metal Substrate is as the solar cell to electrode material.
Therefore, the Cu for preparing of the present invention
2sITO nano-wire array has huge potential using value in area of solar cell, Industrial Catalysis or other scientific domains.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained Cu
2sITO nano-wire array and ITO nano-wire array and In
2o
3the powder x-ray diffraction spectrum of standard P DF card.
Fig. 2 is embodiment 1 gained Cu
2the electron scanning micrograph of SITO nano-wire array.
Fig. 3 is embodiment 1 gained Cu
2sITO nanowire interface place high power transmission electron microscope photo.
Fig. 4 is embodiment 1 gained Cu
2the electron micrograph of the scanning transmission pattern of SITO nano wire and the distribution map of various element.
Fig. 5 is embodiment 1 gained Cu
2sITO nano-wire array is used as IV curve (Fig. 5 (a) and the IPCE curve (Fig. 5 (b)) of quantum dot sensitized solar cell to electrode.
Embodiment
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
Embodiment 1, parcel Cu
2indium tin oxide nanowire array composite (the Cu of S nano particle
2sITO) and application
By Metallic Indium Powder and glass putty according to mol ratio 10:1,800 DEG C are heated in tube furnace, then source region temperature is reacted after 20 minutes and is naturally cooled to room temperature at 800 DEG C, the FTO electro-conductive glass having sputtered Au particle (average grain diameter is 5 nanometers) being placed on position, crystallizing field in tube furnace (temperature is about 400 DEG C) in advance can grow the ITO nano-wire array of certain length.
Select average length be the ITO nano-wire array of 10 microns (wherein, the diameter of nano wire is about 120 nanometers) as the matrix of load, this ITO nano-wire array is placed in the 200mL aqueous solution prepared in advance and (urinates containing 20mM caddy, 66mM ammonium chloride and 140mM sulphur, pH is adjusted to 9.5), react 2 hours at 25 DEG C; Transfer to subsequently 10mL containing 0.5M stannous chloride the aqueous solution in, at 50 DEG C react 5 minutes.Then use natural drying after washed with de-ionized water sample, under an ar atmosphere, 400 DEG C of calcining samples 30 minutes, on ITO nano-wire array, namely wrap up the Cu that thickness is about 20 nanometers finally
2s nano-particle layer, is Cu
2sITO nano-wire array.
Fig. 1 is the present embodiment gained Cu
2sITO nano-wire array and ITO nano-wire array and In
2o
3the powder x-ray diffraction spectrogram of standard P DF card, as known in the figure, can prepare Cu according to the method described above
2sITO composite material.
Fig. 2 is the present embodiment gained Cu
2the electron scanning micrograph of SITO nano-wire array, as seen from the figure, Cu
2s nano particle grows equably on the surface of ITO nano-wire array, Cu
2(particle diameter) diameter of S nano particle is 15 nanometer to 30 nanometers.
Fig. 3 is the present embodiment gained Cu
2the high power transmission electron microscope photo of SITO nano wire, as seen from the figure, Cu
2s nano particle crystallinity is fine, simultaneously Cu
2interface between S and ITO is very good, and lattice line connects together in interface.This epitaxially grown structure obtained is conducive to transmission and the collection of electronics.
Fig. 4 is the present embodiment gained Cu
2the electron micrograph of the scanning transmission pattern of SITO nano wire and the distribution map of various element, can find out more intuitively, Cu from figure
2s nano particle is wrapped in ITO surface uniformly as catalyst unit.
Be further demonstrate that by above-mentioned qualification collection of illustrative plates, method of the present invention can obtain tin indium oxide nano-wire and be surrounded by Cu
2nano-wire array material (the Cu of S nano particle shell
2sITO).
Use Cu prepared by the present embodiment
2sITO nano-wire array material, as to electrode, uses cadmium sulfide and cadmium selenide to be total to the titanium dioxide porous membrane of sensitization, uses 1M vulcanized sodium (Na
2s) and many sulphur electrolyte of preparing of 1M sulphur (S), quantum dot sensitized solar cell device is prepared.Adopt Newport company 450WModel91150 type instrument test IV curve, adopt Newport company IQE-200 test system and test IPCE curve.Adopt metal copper sheet to control incident light area in test process and be prepared as 0.16cm
2, radiation parameter is standard solar irradiation condition (100mW/cm
2).
As shown in Figure 5, be this enforcement gained Cu
2sITO nano-wire array is used as quantum dot sensitized solar cell to the IV curve (5a) of electrode and IPCE curve (5b), can learn, the photoelectric conversion efficiency of this quantum dot sensitized solar cell is 4.06%, monochromatic light conversion efficiency is the highest at 450nm place, reaches 68.3%.
Embodiment 2, parcel Cu
2indium tin oxide nanowire array composite (the Cu of S nano particle
2sITO) and application
Substantially identical with embodiment 1 of concrete preparation method, difference is: select average length be the ITO nano-wire array (wherein, the diameter of nano wire is about 100 nanometers) of 3 microns as the matrix of load, finally prepare Cu
2sITO.
Through Cu prepared by the present embodiment
2sITO is as to electrode, and according to the solar cell device of method assembling quantum dot sensitization in the same manner as in Example 1, and test its photoelectric conversion performance, its photoelectric conversion efficiency is respectively 3.37%.
Embodiment 3, parcel Cu
2indium tin oxide nanowire array composite (the Cu of S nano particle
2sITO) and application
Substantially identical with embodiment 1 of concrete preparation method, difference is: select average length be the ITO nano-wire array (wherein, the diameter of nano wire is about 110 nanometers) of 7 microns as the matrix of load, finally prepare Cu
2sITO.
Through Cu prepared by the present embodiment
2sITO is as to electrode, and according to the solar cell device of method assembling quantum dot sensitization in the same manner as in Example 1, and test its photoelectric conversion performance, its photoelectric conversion efficiency is respectively 3.54%.
Embodiment 4, parcel Cu
2indium tin oxide nanowire array composite (the Cu of S nano particle
2sITO) and application
Substantially identical with embodiment 1 of concrete preparation method, difference is: select ITO electro-conductive glass as conductive substrates, finally prepare Cu
2sITO.
Through Cu prepared by the present embodiment
2sITO is as to electrode, and according to the solar cell device of method assembling quantum dot sensitization in the same manner as in Example 1, and test its photoelectric conversion performance, its photoelectric conversion efficiency is respectively 3.94%.
The Cu of embodiment 5, embodiment 1 preparation
2sITO as the quantum dot sensitized solar cell of dyestuff to electrode
Use the Cu prepared in embodiment 1
2sITO nano-wire array, as to electrode, uses the titanium dioxide porous membrane of dyestuff N719 sensitization as light anode, uses 0.6MPMII, 0.1M guanidine thiocyanate (C
2h
6n
4s), 0.03M iodine (I
2), 0.5M tert .-butylpyridine using the mixed solvent of acetonitrile and valeronitrile 17:3 by volume as electrolyte, prepare the solar cell device that dyestuff is quantum dot sensitized.
After tested, the photoelectric conversion efficiency of the solar cell that above-mentioned dyestuff is quantum dot sensitized is 5.00%.
Comparative example 1,
According to method substantially identical in embodiment 1, Direct precipitation Cu on FTO electro-conductive glass
2s nano particle, then as to electrode material, prepares quantum dot sensitization solar battery according to method in the same manner as in Example 1, and it is 3.04% that test obtains photoelectric conversion efficiency.
Comparative example 2,
According to method substantially identical in embodiment 1, FTO electro-conductive glass grows ITO nano-wire array, then the method for ion sputtering is adopted at the thick Au of ITO nano-wire array surface sputtering one deck 10nm as catalytically-active materials, prepare quantum dot sensitization solar battery according to the method identical with embodiment 1, it is 2.94% that test obtains photoelectric conversion efficiency.
Comparative example 3,
According to method substantially identical in embodiment 1, FTO electro-conductive glass grows ITO nano-wire array, then adopts the method for ion sputtering at the Au of ITO surface sputtering one deck 10nm as catalytically-active materials, prepare electrode material.Prepare quantum dot sensitization solar battery according to the method identical with embodiment 1, it is 2.20% that test obtains photoelectric conversion efficiency.
It should be noted that, above-described embodiment is only used to technical characteristic of the present invention is described, is not used to limit patent claim of the present invention.The reactant related in such as the present embodiment, also can use other reactant, and the length of the ITO nano-wire array adopted in embodiment also can adopt the ITO nano-wire array of other length.But its principle still belongs to patent protection category of the present invention.
Claims (3)
1. an indium tin oxide nanowire array composite, it comprises the tin indium oxide nano-wire array of growth in conductive substrates, and described tin indium oxide nano-wire array is enclosed with cuprous sulfide nano particle;
In described tin indium oxide nano-wire array, the length of tin indium oxide nano-wire is 1 micron ~ 30 microns, and diameter is 50 nanometer ~ 300 nanometers;
The particle diameter of described cuprous sulfide nano particle is 5 nanometer ~ 100 nanometers;
Described conductive substrates is indium oxide tin glass or fluorine-doped tin oxide glass.
2. the preparation method of composite material described in claim 1, comprises the steps:
(1) be catalyst with gold nano grain, by chemical vapour deposition technique, tin indium oxide nano-wire array described in deposition growing in described conductive substrates;
The particle diameter of described gold nano grain is 2 ~ 10 nanometers;
Growing described tin indium oxide nano-wire array indium source used is indium metal and/or indium oxide;
Growing described tin indium oxide nano-wire array Xi Yuan used is metallic tin and/or tin oxide;
The mol ratio of described indium source and described Xi Yuan is 1 ~ 30:1;
Indium source used for the described tin indium oxide nano-wire array of growth and Xi Yuan are heated into gaseous state under the condition of 600 ~ 1000 DEG C;
The growth course of described tin indium oxide nano-wire array is carried out in crystallizing field, and the temperature of described crystallizing field is 300 ~ 550 DEG C, and growth time is 5 ~ 120 minutes;
(2) by chemical bath deposition method, coated CdS nano particle on described tin indium oxide nano-wire array;
The cadmium salt that described chemical bath deposition method uses is cadmium acetate, at least one in caddy, cadmium sulfate and cadmium nitrate;
The sulfosalt that described chemical bath deposition method uses is at least one in sulphur powder, thiocarbamide, thiosemicarbazides and thioacetamide;
The temperature of described chemical bath deposition method is 0 ~ 80 DEG C, and the time is 0.1 ~ 8 hour;
(3) by ion-exchange, described CdS nanoparticle conversion is become Cu
2s nano particle; Then under an inert atmosphere, through calcining and obtain described composite material;
Described ion-exchange comprises the steps:
The tin indium oxide nano-wire array of coated CdS nano particle step (2) obtained is transferred in the aqueous solution of mantoquita, through ion-exchange reactions, becomes Cu by described CdS nanoparticle conversion
2s nano particle;
Described mantoquita is at least one in cuprous acetate, stannous chloride and cuprous sulfate;
The temperature of described ion-exchange reactions is 5 ~ 90 DEG C, and the time is 0.5 ~ 60 minute;
The temperature of described calcining is 250 ~ 500 DEG C, and the time is 10 ~ 60 minutes.
3. indium tin oxide nanowire array composite described in claim 1 as solar cell to the application in electrode.
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| CN103990795B (en) * | 2014-05-30 | 2016-05-25 | 南开大学 | A kind of Ni-Ni2O3Nano composite material |
| CN104143444A (en) * | 2014-07-18 | 2014-11-12 | 中国科学院化学研究所 | Multi-level indium tin oxide nanowire array composite material, preparing method thereof and application in solar cell |
| CN106115771A (en) * | 2016-06-14 | 2016-11-16 | 南京大学 | A kind of In2o3the preparation method that polyhedron micron is brilliant |
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