CN102543471B - 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 nanorod light of CdSe quantum dot sectional composite sensitization anode.
Background technology
In recent years, along with people, the demand of the energy is constantly increased and the continuous decrease of fossil fuel reserves, seek that enrich in a kind of new source, the alternative energy source of 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, and the solar cell research that especially solar energy is converted into electric energy has become the focus of present research.
Quantum dot sensitized solar cell (QDSSC) is the third generation solar cell that occurs the nineties in last century, namely utilizes the base material of inorganic semiconductor quantum dot (QD) the sensitization broad stopband of low energy gap.Quantum dot has very large advantage with respect to dyestuff, and on the one hand, it has quantum confined effect, can regulate the band gap width of quantum dot by 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).If this two large advantage of semiconductor-quantum-point is applied in 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 nanorod light anode mainly contains two kinds: the first is nucleocapsid structure quick ZnO nanorod 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 valence band and the conduction band of stratum nucleare quantum dot); The second is single sensitization ZnO nanorod, and this structure needs long ZnO nanorod.Two kinds of above structures have the pluses and minuses of himself: the advantage of the first structure is that the pairing use of quantum dot can strengthen the Optical Absorption scope, 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 has just limited the kind of choosing of quantum dot greatly, secondly because being unfavorable for the optical excitation electronics that the shell sensitizer produces, the stratum nucleare sensitizer is transferred to rapidly substrate, thereby increased the compound probability of electron-hole, reduced the efficient of battery; The advantage of the second structure is to utilize the large more quantum dot of surface area absorption to increase Optical Absorption intensity, thereby improve the photoelectric conversion efficiency of battery, this kind structure needs ZnO nanorod absorption quantum dot long, that specific area is large, and in the growth course of longer nanometer rods, the adhesion that the bottom of nanometer rods can occur, when length increases surface area, adhesion has reduced again 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 object of the invention is to be total to quick stratum nucleare for nucleocapsid structure and be unfavorable for electric transmission, the nucleocapsid structure problem that the high and longer nanorod growth of Dan Minzhong bottom sticks together to quantum dot sensitized dose of matching request of semiconductor proposes the preparation method of CdS, CdSe quantum dot sectional composite sensitization bilayer ZnO nanorod light anode.
To achieve the above object, the technical solution used in the present invention is:
1) ZnO Seed Layer preparation
At first prepare the ethanolic solution of 5mmol/L zinc acetate, take the ITO electro-conductive glass as substrate, the ethanolic solution of zinc acetate be 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 stove and be warmed up to 400 ℃ of annealing 0.5-1 hour with 3 ℃/min speed, make the ZnO Seed Layer;
2) growth of ground floor ZnO nanorod
Prepare respectively 0.025mol/L hexamethylenetetramine and 0.0125mol/LZn (NO under magnetic agitation
3)
2Each 15ml of solution, at first with Zn (NO
3)
2Solution adds hexamethylenetetramine solution slowly; Be then that 600 polymine dropwise adds with the 0.1ml molecular weight; After polymine disperseed fully, the ammoniacal liquor of getting the 0.7ml mass concentration and be 25-28% dropwise added; Then dropwise add HNO
3Regulate PH to 9.3, make the growth-promoting media of ZnO nanorod; At last growth-promoting media is transferred to and is shifted to an earlier date in preheated reactor, the ZnO Seed Layer is inserted growth solution, in drying baker with 87 ℃ of growths 5-10 hour ZnO nanorods;
3) deposition of CdS quantum dot
Prepare respectively the Na of 50mmol/L
2Cd (the NO of S and 50mmol/L
3)
2Methanol solution, and to prepare corresponding methyl alcohol be cleaning fluid; Adopt again the SILAR method that ZnO nanorod is immersed Na successively
2The methanol solution of S, methyl alcohol, Cd (NO
3)
2Methanol solution, another methyl alcohol in repeatedly, generate the CdS quantum dot in the ZnO nanorod surface reaction;
4) physics or chemical polishing are carried out in the effects on surface ZnO nanorod top that deposits the CdS quantum dot, then adopt the growth immersion method identical with the ground floor ZnO nanorod to carry out the growth of second layer ZnO nanorod;
5) deposition of CdSe quantum dot
At first with the KBH of 0.27g
4Be placed in airtight container, then add 40mL methyl alcohol to make KBH
4Fully dissolving, logical Ar gas is removed the oxygen in container, then adds the SeO of 0.22g in the container
2, at room temperature magnetic agitation reaction obtains the Se of clear
2-Methanol solution; Cd (NO with 0.5g
3)
2Be dissolved in 40mL methyl alcohol and make Cd
2+Methanol solution; The ZnO nanorod of the second layer of having grown is immersed Se successively
2-Methanol solution, methyl alcohol, Cd
2+Methanol solution, repeatedly obtain the double-deck ZnO nanorod light of CdS, CdSe quantum dot sectional composite sensitization 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 nanorod of CdS quantum dot to use the 2000 purpose sand paper CdS quantum dot on nanometer rods top of skimming surface deposition, then cleans 3 minutes in deionized water for ultrasonic.
Described chemical polishing, the ground floor ZnO nanorod that first will deposit the CdS quantum dot immersed in the hexane solution that mass concentration is 0.2% octadecyl trichlorosilane alkane 2 hours, then removed the octadecyl trichlorosilane alkane of nanometer rods top coating in treatment with ultraviolet light 3-5 minute, then the filter paper that iodine and potassium iodide aqueous solution was soaked covers nanometer rods top 2-3 minute removes the CdS quantum dot on nanometer rods top, 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 to carry out polishing to the top of ground floor nanometer rods, prepared CdS, the double-deck ZnO nanorod light of CdSe quantum dot sectional composite sensitization anode, organically combined with advantage Dan Min quick altogether.The ZnO nanorod of growth is conducive to the absorption of sensitization quantum dot, improves photoelectric conversion efficiency, controls density, draw ratio, the interrod spacing of ZnO nanorod by the process conditions of controlling Seed Layer, polymine (PEI) surfactant and growth.The light anode of the quantum dot sectional composite sensitization of the present invention's preparation has the following advantages: first, this structure extension the scope of absorption spectrum, can reduce the electron-hole that nucleocapsid structure causes compound, more meaningfully this structure can select different quantum dot combinations to carry out composite sensitization; The second, utilize the quantum dot be adsorbed on the ZnO nanorod side to suppress the nanometer rods lateral growth, to avoid the bottom adhesion of nanometer rods, also be conducive to the preparation of the nanometer rods light anode of the multilayer more grown simultaneously.If can be good at utilizing this 2 point, just can greatly improve the efficient of quantum dot sensitized ZnO nanorod solar cell.
Description of drawings
Fig. 1 is the double-deck ZnO nanorod light anode construction of CdS, CdSe quantum dot sectional composite sensitization and mechanisms of electronic figure: (a) light anode construction and mechanisms of electronic figure, can realize on 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 ZnO nanorod is modified by CdS, CdSe quantum dot; (c) cosmetic variation of light anode after ground floor ZnO nanorod growth, CdS quantum dot deposition, the growth of second layer ZnO nanorod, four techniques of CdSe quantum dot deposition.The yellow explanation of B in Fig. 1 (c) CdS quantum dot deposition; The light yellow explanation second layer of C nanometer rods in Fig. 1 (c) is partly covered the CdS quantum dot; The deposition of the D kermesinus explanation CdSe quantum dot in Fig. 1 (c).
Fig. 2 is CdS, the double-deck ZnO nanorod light of CdSe quantum dot sectional composite sensitization anode SEM figure, can find out the growth that continues of adopting this technique can realize second layer ZnO nanorod.
Fig. 3 (a), (b) be respectively the battery J-V curve of the double-deck ZnO nanorod light anode absorption spectrum of CdS, CdSe quantum dot sectional composite sensitization and light anode structure: absorption spectrum explanation CdS, CdSe quantum dot sectional sensitization structure make light absorbing scope expand to 600nm; The J-V curve can find out that the fill factor, curve factor (FF=38%) of battery is improved.
Embodiment:
The present invention is further elaborated below in conjunction with accompanying drawing and example.
Embodiment:
1) ZnO Seed Layer preparation
At first prepare the ethanolic solution of 5mmol/L zinc acetate, take the ITO electro-conductive glass as 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 stove and be warmed up to 400 ℃ of annealing 0.5-1 hour with 3 ℃/min speed, make the ZnO Seed Layer;
2) growth of ground floor ZnO nanorod
Prepare respectively 0.025mol/L hexamethylenetetramine and 0.0125mol/LZn (NO under magnetic agitation
3)
2Each 15ml of solution, at first with Zn (NO
3)
2Solution adds hexamethylenetetramine solution slowly; Be then that 600 polymine dropwise adds with the 0.1ml molecular weight; After polymine disperseed fully, the ammoniacal liquor of getting the 0.7ml mass concentration and be 25-28% dropwise added; Then dropwise add HNO
3Regulate PH to 9.3, make the growth-promoting media of ZnO nanorod; At last growth-promoting media is transferred to and is shifted to an earlier date in preheated reactor, the ZnO Seed Layer is inserted growth solution, in drying baker with 87 ℃ of growths 5-10 hour ZnO nanorods;
3) deposition of CdS quantum dot
Prepare respectively the Na of 50mmol/L
2Cd (the NO of S and 50mmol/L
3)
2Methanol solution, and to prepare corresponding methyl alcohol be cleaning fluid; Adopt again the SILAR method that ZnO nanorod is immersed Na successively
2The methanol solution of S, methyl alcohol, Cd (NO
3)
2Methanol solution, another methyl alcohol in repeatedly, generate the CdS quantum dot in the ZnO nanorod surface reaction;
4) physics or chemical polishing are carried out in the effects on surface ZnO nanorod top that deposits the CdS quantum dot, then adopt the growth immersion method identical with the ground floor ZnO nanorod to carry out the growth of second layer ZnO nanorod;
Described physics is scraped, and has the ground floor ZnO nanorod of CdS quantum dot to use the 2000 purpose sand paper CdS quantum dot on nanometer rods top of skimming surface deposition, then cleans 3 minutes in deionized water for ultrasonic.
Described chemical polishing, the ground floor ZnO nanorod that first will deposit the CdS quantum dot immersed in the hexane solution that mass concentration is 0.2% octadecyl trichlorosilane alkane 2 hours, then removed the octadecyl trichlorosilane alkane of nanometer rods top coating in treatment with ultraviolet light 3-5 minute, then the filter paper that iodine and potassium iodide aqueous solution was soaked covers nanometer rods top 2-3 minute removes the CdS quantum dot on nanometer rods top, cleans 3 minutes in deionized water for ultrasonic at last.
5) deposition of CdSe quantum dot
At first with the KBH of 0.27g
4Be placed in airtight container, then add 40mL methyl alcohol to make KBH
4Fully dissolving, logical Ar gas is removed the oxygen in container, then adds the SeO of 0.22g in the container
2, at room temperature magnetic agitation reaction obtains the Se of clear
2-Methanol solution; Cd (NO with 0.5g
3)
2Be dissolved in 40mL methyl alcohol and make Cd
2+Methanol solution; The ZnO nanorod of the second layer of having grown is immersed Se successively
2-Methanol solution, methyl alcohol, Cd
2+Methanol solution, repeatedly obtain the double-deck ZnO nanorod light of CdS, CdSe quantum dot sectional composite sensitization anode in another methyl alcohol.
Claims (4)
1.CdS, the preparation method of the double-deck ZnO nanorod light of CdSe quantum dot sectional composite sensitization anode, it is characterized in that comprising the following steps:
1) ZnO Seed Layer preparation
At first prepare the ethanolic solution of 5mmol/L zinc acetate, take the ITO electro-conductive glass as substrate, the ethanolic solution of zinc acetate be 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 stove and be warmed up to 400 ℃ of annealing 0.5-1 hour with 3 ℃/min speed, make the ZnO Seed Layer;
2) growth of ground floor ZnO nanorod
Prepare respectively 0.025mol/L hexamethylenetetramine and 0.0125mol/LZn (NO under magnetic agitation
3)
2Each 15ml of solution, at first with Zn (NO
3)
2Solution adds hexamethylenetetramine solution slowly; Be then that 600 polymine dropwise adds with the 0.1ml molecular weight; After polymine disperseed fully, the ammoniacal liquor of getting the 0.7ml mass concentration and be 25-28% dropwise added; Then dropwise add HNO
3Regulate PH to 9.3, make the growth-promoting media of ZnO nanorod; At last growth-promoting media is transferred to and is shifted to an earlier date in preheated reactor, the ZnO Seed Layer is inserted growth solution, in drying baker with 87 ℃ of growths 5-10 hour ZnO nanorods;
3) deposition of CdS quantum dot
Prepare respectively the Na of 50mmol/L
2Cd (the NO of S and 50mmol/L
3)
2Methanol solution, and to prepare corresponding methyl alcohol be cleaning fluid; Adopt again the SILAR method that ZnO nanorod is immersed Na successively
2The methanol solution of S, methyl alcohol, Cd (NO
3)
2Methanol solution, another methyl alcohol in repeatedly, generate the CdS quantum dot in the ZnO nanorod surface reaction;
4) physics or chemical polishing are carried out in the effects on surface ZnO nanorod top that deposits the CdS quantum dot, then adopt the growth immersion method identical with the ground floor ZnO nanorod to carry out the growth of second layer ZnO nanorod;
5) deposition of CdSe quantum dot
At first with the KBH of 0.27g
4Be placed in airtight container, then add 40mL methyl alcohol to make KBH
4Fully dissolving, logical Ar gas is removed the oxygen in container, then adds the SeO of 0.22g in the container
2, at room temperature magnetic agitation reaction obtains the Se of clear
2-Methanol solution; Cd (NO with 0.5g
3)
2Be dissolved in 40mL methyl alcohol and make Cd
2+Methanol solution; The ZnO nanorod of the second layer of having grown is immersed Se successively
2-Methanol solution, methyl alcohol, Cd
2+Methanol solution, repeatedly obtain the double-deck ZnO nanorod light of CdS, CdSe quantum dot sectional composite sensitization anode in another methyl alcohol.
2. the preparation method of the double-deck ZnO nanorod light of CdS according to claim 1, CdSe quantum dot sectional composite sensitization 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 the double-deck ZnO nanorod light of CdS according to claim 1, CdSe quantum dot sectional composite sensitization anode, it is characterized in that: described physics polishing, there is the ground floor ZnO nanorod of CdS quantum dot to use the 2000 purpose sand paper CdS quantum dot on nanometer rods top of skimming surface deposition, then cleaned 3 minutes in deionized water for ultrasonic.
4. CdS according to claim 1, the preparation method of the double-deck ZnO nanorod light of CdSe quantum dot sectional composite sensitization anode, it is characterized in that: described chemical polishing, the ground floor ZnO nanorod that first will deposit the CdS quantum dot immersed in the hexane solution that mass concentration is 0.2% octadecyl trichlorosilane alkane 2 hours, then removed the octadecyl trichlorosilane alkane of nanometer rods top coating in treatment with ultraviolet light 3-5 minute, then the filter paper that iodine and potassium iodide aqueous solution was soaked covers nanometer rods top 2-3 minute and removes the CdS quantum dot on nanometer rods top, cleaned 3 minutes in deionized water for ultrasonic at last.
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| CN102760580B (en) * | 2012-07-09 | 2015-06-17 | 湖北大学 | Co-doped CdSe quantum-dot sensitized TiO2 nanorod photoelectrode and preparation method of TiO2 nanorod photoelectrode |
| CN103015166B (en) * | 2012-12-13 | 2014-08-13 | 北京航空航天大学 | Nano-silver antibacterial fabric and preparation method thereof |
| CN103440989B (en) * | 2013-08-27 | 2016-06-01 | 天津儒创新材料科技有限公司 | Inorganic/organic sensitization nanowire solar cells light anode and its preparation method altogether |
| CN104409214A (en) * | 2014-11-19 | 2015-03-11 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for quantum dot modification solar battery photo anode |
| CN105645462B (en) * | 2016-01-06 | 2017-05-17 | 浙江大学城市学院 | Preparation method of CdS/ZnO core-shell-structure nanowires |
| CN106252431A (en) * | 2016-08-11 | 2016-12-21 | 潘忠宁 | A kind of preparation method of CdSZnO core-shell nanometer rod array structure |
| CN106044706A (en) * | 2016-08-16 | 2016-10-26 | 曹健 | CdSe/CdS nanoparticle co-sensitized ZnO photoelectrode preparation method |
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| CN106328381B (en) * | 2016-11-23 | 2018-09-07 | 陕西理工学院 | All solid state quantum dot sensitized solar cell of one kind and preparation method thereof |
| CN107857483B (en) * | 2017-11-01 | 2020-01-31 | 太原理工大学 | Preparation method of titanium dioxide nanosheet films coated with selenium/cadmium sulfide laminated structures |
| CN107988615B (en) * | 2017-11-08 | 2019-07-26 | 常州大学 | A kind of preparation and application of carbonitride modification ZnO/CdS optical anode material |
| CN109326445B (en) * | 2018-11-19 | 2020-04-03 | 河南师范大学 | Nano composite counter electrode for quantum dot sensitized solar cell and preparation method |
| CN110205634B (en) * | 2019-05-24 | 2021-04-20 | 中山大学 | ZnO/ZnS/CdS photo-anode film and preparation method thereof |
| 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 |
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