CN102543471A - Method for preparing CdS and CdSe quantum dot sectional compound sensitized double-layer ZnO nanometer rod photo-anode - Google Patents
Method for preparing CdS and CdSe quantum dot sectional compound sensitized double-layer ZnO nanometer rod photo-anode Download PDFInfo
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Abstract
The invention discloses a method for preparing a CdS and CdSe quantum dot sectional compound sensitized double-layer ZnO nanometer rod photo-anode. The method comprises the following steps: growing a first layer of ZnO nanometer rod by adopting a CBD (Chemical Bath Deposition) method; then depositing CdS quantum dots by adopting an SILAR (Successive Ionic Layer Adsorption And Reaction) method; utilizing physical polishing or chemical polishing to remove the CdS quantum dots from the top of the first layer of nanometer rod; growing a second layer of ZnO nanometer rod by adopting the CBD method again; and finally, depositing CdSe quantum dots by adopting the SILAR method, thereby forming the CdS and CdSe quantum dot sectional compound sensitized double-layer ZnO nanometer rod photo-anode. The method provided by the invention is excellent in repeatability; the lateral growth of the nanometer rods is efficiently restrained by the quantum dots at the bottom; the sectional compound sensitizing of CdS quantum dot single-sensitizing, CdS and CdSe quantum dot co-sensitizing and CdSe quantum dot single-sensitizing is realized; and a quantum dot compound sensitized solar cell prepared according to the method provided by the invention can be used for the wide spectrum absorption and photoelectric conversion of solar energy.
Description
Technical field
The invention belongs to technical field of solar utilization technique, be specifically related to the preparation method of CdS, the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode.
Background technology
In recent years, Along with people's is to the continuous decrease of continuous increase of demands for energy and fossil fuel reserves, and seeking a kind of new source alternative energy source abundant, environmental protection has become one of important topic of present scientific research.Solar energy receives global concern day by day as a kind of inexhaustible natural energy source, especially is converted into solar energy the focus of the present research of solar cell research having become of electric energy.
Quantum dot sensitized solar cell (QDSSC) is the third generation solar cell that occurs the nineties in last century, promptly utilizes the base material of inorganic semiconductor quantum dot (QD) the sensitization broad stopband of low energy gap.Quantum dot has very big advantage with respect to dyestuff, and on the one hand, it has quantum confined effect, can regulate the band gap width of quantum dot through controlling its size and dimension, regulates the scope of absorption spectrum with this; On the other hand, semiconductor-quantum-point has exciton multiplier effect (MEG), and a high-octane photon excitation semiconductor-quantum-point can produce a plurality of electron-hole pairs and (see A.Shabaev, Al.L.Efros, A.J.Nozik, NANO LETTE
-RS, 2006,6, the 22856-22863 page or leaf).If this two big advantage of semiconductor-quantum-point is applied in the solar cell, the theoretical value of QDSSC efficient can reach 44% (M.C.Hanna, A.J.Nozik; Appl.Phys.2006; 100,074510), the theoretical value 32.9% than crystal silicon solar energy battery is high a lot.Therefore, no matter be at cost or using, the potentiality of the development of QDSSC are huge.
At present; The structure of quantum dot sensitized ZnO nanometer rods light anode mainly contains two kinds: first kind is nucleocapsid structure quick ZnO nanometer rods altogether, and this structure needs the band gap of two kinds of semiconductor-quantum-points to form notch cuttype (valence band of shell quantum dot and conduction band are higher than the valence band and the conduction band of stratum nucleare quantum dot); Second kind is single sensitization ZnO nanometer rods, and this structure needs long ZnO nanometer rods.Two kinds of above structures all have the pluses and minuses of himself: the advantage of first kind of structure is that the absorption region that can strengthen light is used in the pairing of quantum dot; Thereby improve the photoelectric conversion efficiency of battery; What but this kind structure needed is the semiconductor-quantum-point pairing use that band gap is notch cuttype; This just big limitations quantum dot choose kind; Secondly be transferred to substrate apace because the stratum nucleare sensitizer is unfavorable for the optical excitation electronics that the shell sensitizer produces, thereby increased the compound probability in electronics-hole, reduce the efficient of battery; The advantage of second kind of structure is to utilize big surface area to adsorb the absorption intensity that more quantum dot increases light; Thereby improve the photoelectric conversion efficiency of battery; This kind structure needs long, that specific area is big ZnO nanometer rods absorption quantum dot; And in the growth course of longer nanometer rods, the adhesion that the bottom of nanometer rods can take place, adhesion had reduced surface area again when length increased surface area.Comprehensive for these two kinds of structure pluses and minuses if can overcome its shortcoming, inherited both advantages, and the efficient of so quantum dot sensitized battery just might be greatly enhanced.
The content of invention
The objective of the invention is to be total to quick stratum nucleare and be unfavorable for electric transmission to nucleocapsid structure; The problem that nucleocapsid structure is high to quantum dot sensitized dose of matching request of semiconductor and the longer nanorod growth of Dan Minzhong bottom sticks together, the preparation method of proposition CdS, the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode.
In order to reach above-mentioned purpose, the technical scheme that the present invention adopts is:
1) ZnO Seed Layer preparation
At first preparing the ethanolic solution of 5mmol/L zinc acetate, is substrate with the ITO electro-conductive glass, the ethanolic solution of zinc acetate is spin-coated in the substrate of ITO electro-conductive glass, then in Muffle furnace 300 ℃ of heat treatments 20 minutes, repeat spin coating, heat treatment 2 times; Put it at last in the stove and be warmed up to 400 ℃ of annealing 0.5-1 hour, make the ZnO Seed Layer with 3 ℃/min speed;
2) growth of ground floor ZnO nanometer rods
Under magnetic agitation, prepare 0.025mol/L hexamethylenetetramine and 0.0125mol/LZn (NO respectively
3)
2Each 15ml of solution, at first with Zn (NO
3)
2Solution adds hexamethylenetetramine solution slowly; Be that 600 polymine dropwise adds then with the 0.1ml molecular weight; After treating that polymine disperses fully, the ammoniacal liquor of getting the 0.7ml mass concentration and be 25-28% dropwise adds; Dropwise add HNO then
3Regulate PH to 9.3, make the growth-promoting media of ZnO nanometer rods; At last growth-promoting media is transferred in the good agitated reactor of preheating in advance, the ZnO Seed Layer is inserted growth solution, in drying baker, got the ZnO nanometer rods in 5-10 hour with 87 ℃ of growths;
3) deposition of CdS quantum dot
Prepare the Na of 50mmol/L respectively
2Cd (the NO of S and 50mmol/L
3)
2Methanol solution, and to prepare corresponding methyl alcohol be cleaning fluid; Adopt the SILAR method that the ZnO nanometer rods is immersed Na successively again
2The methanol solution of S, methyl alcohol, Cd (NO
3)
2Methanol solution, another methyl alcohol in repeat repeatedly, generate the CdS quantum dot in the reaction of ZnO nanorod surfaces;
4) physics or chemical polishing are carried out in the ZnO nanometer rods top that the surface is deposited the CdS quantum dot, adopt the growth immersion method identical with ground floor ZnO nanometer rods to carry out the growth of second layer ZnO nanometer rods then;
5) deposition of CdSe quantum dot
At first with the KBH of 0.27g
4Place airtight container, add 40mL methyl alcohol again and make KBH
4Fully dissolving, logical Ar gas is removed the oxygen in the container, adds the SeO of 0.22g then in the container
2, magnetic agitation reaction at room temperature obtains the Se of clear
2-Methanol solution; Cd (NO with 0.5g
3)
2Be dissolved in the 40mL methyl alcohol and make Cd
2+Methanol solution; The ZnO nanometer rods of the second layer of having grown is immersed Se successively
2-Methanol solution, methyl alcohol, Cd
2+Methanol solution, repeat repeatedly to obtain the double-deck ZnO nanometer rods of CdS, CdSe quantum dot segmentation composite sensitization light anode in another methyl alcohol.
Described spin coating is adopted 2000rmp, is carried out the 30s spin coating 5 times.
Described physics is scraped, and has the ground floor ZnO nanometer rods of CdS quantum dot to use the skim CdS quantum dot on nanometer rods top of 2000 purpose sand paper surface deposition, cleans 3 minutes in deionized water for ultrasonic again.
Described chemical polishing; The ground floor ZnO nanometer rods that will deposit the CdS quantum dot earlier immersed in the hexane solution that mass concentration is 0.2% octadecyl trichlorosilane 2 hours; Then removed the octadecyl trichlorosilane that the nanometer rods top coats in treatment with ultraviolet light 3-5 minute; The filter paper that then iodine and potassium iodide aqueous solution was soaked covers the CdS quantum dot that the nanometer rods top was removed at the nanometer rods top in 2-3 minute, cleans 3 minutes in deionized water for ultrasonic at last.
The present invention adopts chemical bath deposition (CBD) method growing ZnO nanorod; Adopt SILAR method deposition CdS, CdSe quantum dot; Adopt physics or chemical method that the top of ground floor nanometer rods is polished; Prepared CdS, the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode, organically combined with advantage Dan Min quick altogether.The ZnO nanometer rods of growth helps the absorption of sensitization quantum dot, improves photoelectric conversion efficiency, controls density, draw ratio, the interrod spacing of ZnO nanometer rods through the process conditions of control Seed Layer, polymine (PEI) surfactant and growth.The light anode of the quantum dot segmentation composite sensitization of the present invention's preparation has the following advantages: first; This structural extended the scope of absorption spectrum; Can reduce electronics-hole-recombination that nucleocapsid structure causes, more meaningfully this structure can be selected different quantum dot combination carrying out composite sensitizations; The second, utilize the quantum dot that is adsorbed on ZnO nanometer rods side to suppress the nanometer rods lateral growth, to avoid the bottom adhesion of nanometer rods, also help the preparation of the nanometer rods light anode of longer multilayer simultaneously.If can be good at utilizing this 2 point, just can improve the efficient of quantum dot sensitized ZnO nanometer rods solar cell greatly.
Description of drawings
Fig. 1 is double-deck ZnO nanometer rods light anode construction of CdS, CdSe quantum dot segmentation composite sensitization and mechanisms of electronic figure: (a) light anode construction and mechanisms of electronic figure, can realize on the principle that CdS quantum dot Dan Min, CdS and CdSe quantum dot are total to the segmentation composite sensitization of quick and CdSe quantum dot Dan Min; (b) energy band diagram after the ZnO nanometer rods is modified by CdS, CdSe quantum dot; (c) cosmetic variation of light anode after ground floor ZnO nanorod growth, CdS quantum dot deposition, second layer ZnO nanorod growth, four technologies of CdSe quantum dot deposition.The yellow explanation of B among Fig. 1 (c) CdS quantum dot deposition; The light yellow explanation second layer of C nanometer rods among Fig. 1 (c) is partly covered the CdS quantum dot; The deposition of the D kermesinus explanation CdSe quantum dot among Fig. 1 (c).
Fig. 2 is CdS, the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode SEM figure, can find out the growth that continues of adopting this technology can realize second layer ZnO nanometer rods.
Fig. 3 (a), (b) be the battery J-V curve of double-deck ZnO nanometer rods light anode absorption spectrum of CdS, CdSe quantum dot segmentation composite sensitization and light anode structure respectively: absorption spectrum explanation CdS, CdSe quantum dot segmentation sensitization structure make light absorbing range expansion to 600nm; The J-V curve can find out that the fill factor, curve factor (FF=38%) of battery is improved.
Embodiment:
Below in conjunction with accompanying drawing and instance the present invention is done further elaboration.
Embodiment:
1) ZnO Seed Layer preparation
At first prepare the ethanolic solution of 5mmol/L zinc acetate; With the ITO electro-conductive glass is substrate; The ethanolic solution of zinc acetate is spin-coated in the substrate of ITO electro-conductive glass; Spin coating is adopted 2000rmp, is carried out the 30s spin coating 5 times, then in Muffle furnace 300 ℃ of heat treatments 20 minutes, repeat spin coating, heat treatment 2 times; Put it at last in the stove and be warmed up to 400 ℃ of annealing 0.5-1 hour, make the ZnO Seed Layer with 3 ℃/min speed;
2) growth of ground floor ZnO nanometer rods
Under magnetic agitation, prepare 0.025mol/L hexamethylenetetramine and 0.0125mol/LZn (NO respectively
3)
2Each 15ml of solution, at first with Zn (NO
3)
2Solution adds hexamethylenetetramine solution slowly; Be that 600 polymine dropwise adds then with the 0.1ml molecular weight; After treating that polymine disperses fully, the ammoniacal liquor of getting the 0.7ml mass concentration and be 25-28% dropwise adds; Dropwise add HNO then
3Regulate PH to 9.3, make the growth-promoting media of ZnO nanometer rods; At last growth-promoting media is transferred in the good agitated reactor of preheating in advance, the ZnO Seed Layer is inserted growth solution, in drying baker, got the ZnO nanometer rods in 5-10 hour with 87 ℃ of growths;
3) deposition of CdS quantum dot
Prepare the Na of 50mmol/L respectively
2Cd (the NO of S and 50mmol/L
3)
2Methanol solution, and to prepare corresponding methyl alcohol be cleaning fluid; Adopt the SILAR method that the ZnO nanometer rods is immersed Na successively again
2The methanol solution of S, methyl alcohol, Cd (NO
3)
2Methanol solution, another methyl alcohol in repeat repeatedly, generate the CdS quantum dot in the reaction of ZnO nanorod surfaces;
4) physics or chemical polishing are carried out in the ZnO nanometer rods top that the surface is deposited the CdS quantum dot, adopt the growth immersion method identical with ground floor ZnO nanometer rods to carry out the growth of second layer ZnO nanometer rods then;
Described physics is scraped, and has the ground floor ZnO nanometer rods of CdS quantum dot to use the skim CdS quantum dot on nanometer rods top of 2000 purpose sand paper surface deposition, cleans 3 minutes in deionized water for ultrasonic again.
Described chemical polishing; The ground floor ZnO nanometer rods that will deposit the CdS quantum dot earlier immersed in the hexane solution that mass concentration is 0.2% octadecyl trichlorosilane 2 hours; Then removed the octadecyl trichlorosilane that the nanometer rods top coats in treatment with ultraviolet light 3-5 minute; The filter paper that then iodine and potassium iodide aqueous solution was soaked covers the CdS quantum dot that the nanometer rods top was removed at the nanometer rods top in 2-3 minute, cleans 3 minutes in deionized water for ultrasonic at last.
5) deposition of CdSe quantum dot
At first with the KBH of 0.27g
4Place airtight container, add 40mL methyl alcohol again and make KBH
4Fully dissolving, logical Ar gas is removed the oxygen in the container, adds the SeO of 0.22g then in the container
2, magnetic agitation reaction at room temperature obtains the Se of clear
2-Methanol solution; Cd (NO with 0.5g
3)
2Be dissolved in the 40mL methyl alcohol and make Cd
2+Methanol solution; The ZnO nanometer rods of the second layer of having grown is immersed Se successively
2-Methanol solution, methyl alcohol, Cd
2+Methanol solution, repeat repeatedly to obtain the double-deck ZnO nanometer rods of CdS, CdSe quantum dot segmentation composite sensitization light anode in another methyl alcohol.
Claims (4)
1.CdS, the preparation method of the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode, it is characterized in that may further comprise the steps:
1) ZnO Seed Layer preparation
At first preparing the ethanolic solution of 5mmol/L zinc acetate, is substrate with the ITO electro-conductive glass, the ethanolic solution of zinc acetate is spin-coated in the substrate of ITO electro-conductive glass, then in Muffle furnace 300 ℃ of heat treatments 20 minutes, repeat spin coating, heat treatment 2 times; Put it at last in the stove and be warmed up to 400 ℃ of annealing 0.5-1 hour, make the ZnO Seed Layer with 3 ℃/min speed;
2) growth of ground floor ZnO nanometer rods
Under magnetic agitation, prepare 0.025mol/L hexamethylenetetramine and 0.0125mol/LZn (NO respectively
3)
2Each 15ml of solution, at first with Zn (NO
3)
2Solution adds hexamethylenetetramine solution slowly; Be that 600 polymine dropwise adds then with the 0.1ml molecular weight; After treating that polymine disperses fully, the ammoniacal liquor of getting the 0.7ml mass concentration and be 25-28% dropwise adds; Dropwise add HNO then
3Regulate PH to 9.3, make the growth-promoting media of ZnO nanometer rods; At last growth-promoting media is transferred in the good agitated reactor of preheating in advance, the ZnO Seed Layer is inserted growth solution, in drying baker, got the ZnO nanometer rods in 5-10 hour with 87 ℃ of growths;
3) deposition of CdS quantum dot
Prepare the Na of 50mmol/L respectively
2Cd (the NO of S and 50mmol/L
3)
2Methanol solution, and to prepare corresponding methyl alcohol be cleaning fluid; Adopt the SILAR method that the ZnO nanometer rods is immersed Na successively again
2The methanol solution of S, methyl alcohol, Cd (NO
3)
2Methanol solution, another methyl alcohol in repeat repeatedly, generate the CdS quantum dot in the reaction of ZnO nanorod surfaces;
4) physics or chemical polishing are carried out in the ZnO nanometer rods top that the surface is deposited the CdS quantum dot, adopt the growth immersion method identical with ground floor ZnO nanometer rods to carry out the growth of second layer ZnO nanometer rods then;
5) deposition of CdSe quantum dot
At first with the KBH of 0.27g
4Place airtight container, add 40mL methyl alcohol again and make KBH
4Fully dissolving, logical Ar gas is removed the oxygen in the container, adds the SeO of 0.22g then in the container
2, magnetic agitation reaction at room temperature obtains the Se of clear
2-Methanol solution; Cd (NO with 0.5g
3)
2Be dissolved in the 40mL methyl alcohol and make Cd2
+Methanol solution; The ZnO nanometer rods of the second layer of having grown is immersed Se successively
2-Methanol solution, methyl alcohol, Cd
2+Methanol solution, repeat repeatedly to obtain the double-deck ZnO nanometer rods of CdS, CdSe quantum dot segmentation composite sensitization light anode in another methyl alcohol.
2. the preparation method of CdS according to claim 1, the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode, it is characterized in that: described spin coating is adopted 2000rmp, is carried out the 30s spin coating 5 times.
3. the preparation method of CdS according to claim 1, the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode; It is characterized in that: described physics is scraped; There is the ground floor ZnO nanometer rods of CdS quantum dot to use the skim CdS quantum dot on nanometer rods top of 2000 purpose sand paper surface deposition, cleaned 3 minutes in deionized water for ultrasonic again.
4. the preparation method of CdS according to claim 1, the double-deck ZnO nanometer rods of CdSe quantum dot segmentation composite sensitization light anode; It is characterized in that: described chemical polishing; The ground floor ZnO nanometer rods that will deposit the CdS quantum dot earlier immersed in the hexane solution that mass concentration is 0.2% octadecyl trichlorosilane 2 hours; Then removed the octadecyl trichlorosilane that the nanometer rods top coats in treatment with ultraviolet light 3-5 minute; The filter paper that then iodine and potassium iodide aqueous solution was soaked covers the CdS quantum dot that the nanometer rods top was removed at the nanometer rods top in 2-3 minute, cleans 3 minutes in deionized water for ultrasonic at last.
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| CN102760580A (en) * | 2012-07-09 | 2012-10-31 | 湖北大学 | Co-doped CdSe quantum-dot sensitized TiO2 nanorod photoelectrode and preparation method of TiO2 nanorod photoelectrode |
| CN103015166A (en) * | 2012-12-13 | 2013-04-03 | 北京航空航天大学 | Nano-silver antibacterial fabric and preparation method thereof |
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| CN110205634B (en) * | 2019-05-24 | 2021-04-20 | 中山大学 | ZnO/ZnS/CdS photo-anode film and preparation method thereof |
| CN113281390A (en) * | 2021-07-02 | 2021-08-20 | 萍乡学院 | BiSeTe/CdS nano-rod material, photo-anode, preparation method and Cu thereof2+Applications on detection |
| CN113281390B (en) * | 2021-07-02 | 2023-05-30 | 萍乡学院 | BiSeTe/CdS nano rod material, photo-anode, preparation method and Cu thereof 2+ Application to detection |
| CN113736450A (en) * | 2021-09-30 | 2021-12-03 | 江南大学 | Chiral nanorod film with circular polarization fluorescence |
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