CN113707461A - CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite, cell and preparation method of CdSe/CdSe quantum dot sensitized solar cell photo-anode - Google Patents
CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite, cell and preparation method of CdSe/CdSe quantum dot sensitized solar cell photo-anode Download PDFInfo
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- 150000001450 anions Chemical class 0.000 claims description 4
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- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 4
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- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical group CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 3
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2054—Light-sensitive devices comprising a semiconductor electrode comprising AII-BVI compounds, e.g. CdTe, CdSe, ZnTe, ZnSe, with or without impurities, e.g. doping materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2004—Light-sensitive devices characterised by the electrolyte, e.g. comprising an organic electrolyte
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Photovoltaic Devices (AREA)
- Hybrid Cells (AREA)
Abstract
The invention relates to a CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite, a cell and a preparation method thereof. Calcining zinc-tin hydrotalcite to generate mixed metal oxide, coating the mixed metal oxide on conductive glass to form a porous film, and sequentially loading CdS and CdSe quantum dots to form a photo-anode; and then the quantum dot sensitized solar cell is assembled with a polysulfide electrolyte and a CuS counter electrode to form a sandwich structure. The molar ratio of zinc to tin of the hydrotalcite-like compound is 7-11: 1, the adsorption cycle of CdS quantum dots is 9-13 times, and the CdSe quantum dots are deposited once. The CdS/CdSe quantum dot sensitized solar cell has the advantages of good photoelectric conversion efficiency, simple preparation method and low cost.
Description
Technical Field
The invention relates to a CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite, a solar cell and a preparation method thereof, and belongs to the technical field of solar cells.
Background
Quantum dot-sensitized solar cells (QDSSCs) are a new type of solar cell, and are receiving much attention because of their high theoretical efficiency. Limited by the photoanode material and charge recombination, its practical efficiency is low. 2011 reported in literature, Zn2SnO4Nano particles are used as a photo-anode material of a quantum dot sensitized solar cell, and Zn is prepared by chemical bath deposition2SnO4The CdS quantum dots of the electrode are sensitized, the ZnS layer is optimized, and the photoelectric conversion efficiency of 0.228% is obtained. The purpose of the research is to lead the ternary oxide Zn containing zinc and tin2SnO4Applied to quantum dot sensitized solar cells, but is limited by Zn2SnO4The band gap, the morphology and the components of the cell are not adjustable, and the photoelectric conversion efficiency of the cell is low.
CN103854869A discloses a manganin doped CdS quantum dot sensitizer for solar cells and a preparation method thereof. According to the method, Mn impurity atoms and Cu impurity atoms are respectively doped into CdS quantum dots to serve as sensitizing agents, and the quantum dot sensitized solar cell is assembled. By introducing impurity atoms Mn and Cu, a middle energy level is formed in a forbidden band of CdS, and photoresponse is enhanced, so that the short-circuit current density and the photoelectric conversion efficiency of the solar cell are improved, and the short-circuit current density is 6.46mA cm-2And the photoelectric conversion efficiency can reach 1.02%. However, the defect that the light absorption range is limited due to the wider forbidden band of CdS is difficult to compensate by the doped intermediate energy level, and the short-circuit current density and the photoelectric conversion efficiency of the battery are improved slightly.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite and a preparation method thereof. The porous nano semiconductor film of the mixed metal oxide is formed by adopting zinc-tin hydrotalcite, and CdS and CdSe are adopted for sequential sensitization, so that the defect that the single sensitization light absorption range is limited is overcome.
In a second aspect, the invention also provides a CdS/CdSe quantum dot sensitized solar cell based on the zinc-tin hydrotalcite and a preparation method thereof.
In a third aspect, the invention also provides an application of the CdS/CdSe quantum dot sensitized solar cell based on the zinc-tin hydrotalcite.
The technical scheme of the invention is as follows:
a CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite comprises conductive glass, a semiconductor film and CdS and CdSe quantum dots sequentially loaded on the semiconductor film; wherein the content of the first and second substances,
the semiconductor film is a nano-porous semiconductor film of mixed metal oxide formed by calcining zinc-tin hydrotalcite, and the molar ratio of zinc to tin in the zinc-tin hydrotalcite is 7-11: 1;
the CdS and CdSe quantum dots sequentially loaded on the semiconductor film are obtained by firstly carrying out CdS quantum dot adsorption circulation on the semiconductor film for 8-14 times and then carrying out CdSe quantum dot deposition for one time.
According to the optimized CdS and CdSe quantum dots sequentially loaded on the semiconductor film, the CdS quantum dot adsorption cycle is carried out on the semiconductor film for 9-13 times, and then the CdSe quantum dot deposition is carried out once. The deposition time of the CdSe quantum dots is 3-5 hours; most preferably, the CdSe quantum dots are deposited once for 4 hours. The balance of the adsorption amounts of CdS and CdSe quantum dots is very important, the light absorption is insufficient due to the small adsorption amount, the charge recombination is aggravated due to the excessive adsorption amount, and when the difference between the adsorption amounts of the two quantum dots is large, the improvement of the light absorption and the inhibition of the charge recombination are not facilitated.
More preferably, the CdS quantum dot adsorption is to immerse the semiconductor film into a Cd-containing cation solution, take out, clean, dry and immerse the semiconductor film into an S-containing anion solution, and the sequence is not limited. The cation solution is preferably 0.05-0.3M Cd (NO)3)2The S anion-containing solution is 0.05-0.3M of Na2S ethanol aqueous solution.
According to the invention, the molar ratio of zinc to tin in the zinc-tin hydrotalcite is preferably 8-10: 1.
Preferably, according to the invention, the conductive glass is a fluorine-doped tin oxide conductive glass. More preferably, the conductive glass is fluorine-doped tin oxide conductive glass with the sheet resistance of 10-15 omega.
According to the invention, the preparation method of the CdS/CdSe quantum dot sensitized solar cell photo-anode based on the zinc-tin hydrotalcite comprises the following steps:
(1) calcining zinc-tin hydrotalcite powder at 400-700 ℃ to obtain a zinc-tin mixed metal oxide;
(2) preparing the prepared zinc-tin mixed metal oxide into slurry by using a solvent and an auxiliary agent, coating the slurry on conductive glass to form a film, then placing the film in a muffle furnace, heating to 400-500 ℃, and keeping the temperature for 20-40 min to obtain a nano porous semiconductor film of the zinc-tin mixed metal oxide;
(3) placing the zinc-tin mixed metal oxide nano-porous film in Cd (NO)3)2Adding the mixture into the solution for 0.5-2 min, taking out, washing with ethanol, drying, and adding Na2Taking out the S solution after 0.5-2 min, cleaning with ethanol and drying, wherein the above processes are a cycle, and the cycle is totally 8-14 times to obtain the CdS quantum dot sensitized zinc-tin mixed metal oxide;
(4) immersing the CdS quantum dot sensitized zinc-tin mixed metal oxide prepared in the step (3) in Na with the same volume2SeSO3Aqueous solution, Cd (NO)3)2And depositing the mixed solution consisting of the aqueous solution and the sodium nitrilotriacetate aqueous solution at room temperature in a dark place for 3-5 hours to obtain the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide, namely the CdS/CdSe quantum dot sensitized solar cell photo-anode.
Preferably, in step (1), the size of the zinc-tin mixed metal oxide is 100 to 500 nm. The nano porous semiconductor film prepared by the zinc-tin mixed metal oxide with the size has larger specific surface area, pores are easy to block when the size is too small, electrolyte permeation is not facilitated, and the specific surface area is reduced when the size is too large, so that quantum dot adsorption is not facilitated.
Preferably, in the step (1), the calcination of the zinc-tin hydrotalcite powder is carried out in a muffle furnace.
Preferably, in step (2), the solvent is terpineol or silicone oil. The auxiliary agent is ethyl cellulose or butyl cellulose.
According to the invention, in the step (2), the mass-to-volume ratio of the zinc-tin mixed metal oxide to the solvent is 1: 4-5, and the unit is g: mL. The mass volume ratio of the zinc-tin mixed metal oxide to the auxiliary agent is 1: 9-12, and the unit g: mL.
According to the invention, in the step (2), the temperature rise is preferably carried out at a speed of 3-6 ℃/min.
Preferably, in step (1), the zinc-tin hydrotalcite powder is prepared by urea hydrolysis. Can be prepared by referring to the method for preparing the metal hydrotalcite by the urea method in the prior art. The present invention provides a preferred method as follows: taking Zn (NO) according to the molar ratio of zinc to tin of 7-11: 13)2·6H2O、SnCl4·5H2O, and an appropriate amount of CO (NH)2)2Dissolving in deionized water, heating in an oil bath at 95-100 ℃ for 20-26 h, and cleaning, filtering, drying and grinding reaction products to obtain the zinc-tin hydrotalcite powder.
The CdS/CdSe quantum dot sensitized solar cell photo-anode is used for preparing a quantum dot sensitized solar cell and is used as an anode material.
A CdS/CdSe quantum dot sensitized solar cell based on zinc-tin hydrotalcite is characterized in that a sandwich structure is formed by a photo-anode, an electrolyte and a counter electrode; wherein the content of the first and second substances,
the photo-anode is the CdS/CdSe quantum dot sensitized solar cell photo-anode;
the electrolyte is polysulfide electrolyte composed of Na2S·9H2Dissolving O and sublimed sulfur in deionized water to obtain the product;
the counter electrode is a CuS counter electrode.
According to the invention, the CuS counter electrode is formed by immersing conductive glass in CuSO4、Na2S2O3And CH4N2And (3) preparing a mixed aqueous solution of O at the temperature of 60-80 ℃ in a dark place for 2-3 hours. Further preferably, the conductive glass is fluorine-doped tin oxide conductive glass; preferably, the fluorine-doped tin oxide conductive glass has a sheet resistance of 5-8 omega.
A preparation method of CdS/CdSe quantum dot sensitized solar cells based on zinc-tin hydrotalcite comprises the following steps:
1) preparation of a CdS/CdSe quantum dot sensitized solar cell photo-anode, as in the method of the previous section of the invention;
2) preparation of polysulfide electrolyte
Taking Na according to the molar ratio of 1-3: 12S·9H2Dissolving O and sulfur in deionized water to make Na2S·9H2Stirring at 45-55 ℃ with the molar concentration of O being 1-3 mol/L to obtain polysulfide electrolyte;
3) preparation of CuS counter electrode
Vertically placing fluorine-doped tin oxide conductive glass in a container, and adding a solution containing 0.05-0.2M of CuSO4、0.2～0.8M Na2S2O3And 0.2 to 0.8M CH4N2O, enabling the mixed water solution to submerge the conductive glass, keeping away from light at the temperature of 60-80 ℃ for 2-3 hours, taking out, cleaning and drying to obtain a CuS counter electrode;
4) assembly
And sequentially assembling the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide photo-anode, the polysulfide electrolyte and the CuS counter electrode into a sandwich-structured battery by using a heat-sealing film.
Preferably, in the step 2) of preparing the polysulfide electrolyte, the sulfur is sublimed sulfur.
Preferably, in the step 2) of preparing the polysulfide electrolyte, Na is added in an equimolar amount2S·9H2Dissolving O and sulfur in deionized water to prepare 1M Na2S and 1M aqueous solution of sublimed sulphur.
Preferably, in the step 3) of preparing the CuS counter electrode, the mixed aqueous solution contains 0.08-0.1 mcusso4、0.4～0.5M Na2S2O3And 0.4 to 0.5M CH4N2O。
Preferably, in the step 3) of preparing the CuS counter electrode, the conductive glass is fluorine-doped tin oxide conductive glass with a sheet resistance of 5-8 Ω.
The above-described preparation methods of the present invention are not particularly limited, and can be performed according to the prior art.
XRD, SEM, TEM and UV-vis analysis of the zinc-tin hydrotalcite, the zinc-tin mixed metal oxide and the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide respectively show that the zinc-tin mixed metal oxide and the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide based on the hydrotalciteThe CdS/CdSe quantum dot sensitizer is successfully prepared, and the photoanode of the CdS/CdSe quantum dot sensitized solar cell has good absorption in ultraviolet and visible light ranges. J-V test is carried out on the assembled battery, good short-circuit current density, open-circuit voltage and photoelectric conversion efficiency are obtained, the battery efficiency is 3.31% when CdS quantum dots are absorbed and circulated for 11 times and CdSe quantum dots are deposited for 4 hours in example 1, and the short-circuit current density is 17.41mA cm-2。
Preparing hydrotalcite-like compound with a zinc-tin molar ratio of 7-11: 1 by a urea hydrolysis method, calcining to generate mixed metal oxide, coating the mixed metal oxide on conductive glass to form a porous film, utilizing continuous ionic layer adsorption reaction and chemical water bath deposition to sequentially load CdS quantum dots and CdSe quantum dots, wherein adsorption cycle of the CdS quantum dots is 8-14 times, deposition time of the CdSe quantum dots is 3-5 hours, and assembling the CdS quantum dots, the polysulfide electrolyte and a CuS counter electrode into a quantum dot sensitized solar cell with a sandwich structure.
The CdS/CdSe quantum dot sensitized solar cell is applied to converting solar energy into electric energy. In particular, the flexible power generation device is used for solar power generation on the outer surface of a building, a power supply of low-power electronic devices or a flexible power generation product matched with textiles.
The CdS/CdSe quantum dot sensitized solar cell can be used for solar power generation on the outer surface of a building, a power supply of a low-power electronic device or a flexible power generation product matched with a textile fabric due to the light transmittance and flexibility of the film material.
The invention has the technical characteristics and excellent effects that:
1. the invention uses zinc-tin hydrotalcite to calcine to generate mixed metal oxide, which is used as a nano semiconductor film of a photo-anode, and the nano semiconductor film, after being double sensitized by CdS and CdSe, is assembled with a polysulfide electrolyte and a CuS counter electrode to form a quantum dot sensitized solar cell. Wherein, the zinc-tin Hydrotalcite (HTlc) is a layered double hydroxide, and forms a porous Mixed Metal Oxide (MMO) after calcination, the adjustable proportion of zinc and tin is helpful for optimizing the electron transport performance of the photo-anode, and the sheet structure has a larger specific surface area and is beneficial to the adsorption of a sensitizer (CdS/CdSe). The combination of the semiconductor oxide and the quantum dot sensitizer has important significance for improving the performance of the battery.
2. According to the invention, CdS and CdSe are adopted for sequential sensitization, so that better energy level matching is formed, and the defect of limited single sensitization light absorption range is overcome. The CdS quantum dot adsorption cycle is carried out on the nano semiconductor film of the porous mixed metal oxide for 8-14 times, then the CdSe quantum dot deposition is carried out once, and the sensitization sequence can form good energy level matching of CdS and CdSe and is beneficial to transmission of photo-generated charges. The inventor unexpectedly finds that the sensitization sequence of CdS and CdSe cannot be changed, otherwise the adsorbed CdSe conduction band bottom is lower, which is not beneficial to injecting photo-generated electrons into the film in the sensitizer; and the valence band top of the adsorbed CdS is lower, so that the transmission of photogenerated holes in the CdSe can be blocked.
3. The CdS/CdSe quantum dot sensitized solar cell based on the zinc-tin hydrotalcite has better photoelectric conversion efficiency, the photoelectric conversion efficiency of the cell is improved to about 3 percent and can reach 3.31 percent, and the short-circuit current density is increased to 17.41mA cm-2And is improved by about three times compared with the prior art. The ratio of zinc to tin is controlled to be 7-11: 1, the problems of quantum dot adsorption and charge transmission are well balanced, light absorption is improved, and charge recombination is inhibited.
4. The preparation method is simple and low in cost. The zinc-tin ratio in the mixed metal oxide based on the zinc-tin hydrotalcite is adjustable, the CdS/CdSe quantum dot content is controllable, and solar cells with different light absorption intensities can be prepared to adapt to application in different environments.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a zinc-tin hydrotalcite prepared in example 1 (Zn-Sn HTlc), a zinc-tin mixed metal oxide (Zn-Sn MMO), and a CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide (Zn-Sn MMO/CdS/CdSe). The abscissa is 2 θ (°), and the ordinate is intensity (arbitrary unit).
Fig. 2 is a Scanning Electron Microscope (SEM) picture and (d) elemental distribution diagram of (a) a zinc-tin hydrotalcite-like compound, (b) a zinc-tin mixed metal oxide, and (c) a CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide prepared in example 1.
FIG. 3 is a Transmission Electron Microscope (TEM) image of a CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide prepared in example 1.
FIG. 4 is a graph of the ultraviolet-visible light absorption (UV-vis) of CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxides prepared in examples 1-5; the graphs labeled 1-5 in the figures correspond to examples 1-5. The abscissa is the wavelength (nm) and the ordinate is the absorbance (arbitrary unit).
FIG. 5 is a J-V test curve of CdS/CdSe quantum dot sensitized solar cells based on zinc-tin hydrotalcite-like compounds prepared in examples 1-5; the curves labeled 1-5 in the figures correspond to examples 1-5. The abscissa is the voltage (V) and the ordinate is the current density (mA cm)-2)。
Fig. 6 is a schematic view of a solar cell assembly structure according to the present invention. The method comprises the following steps of 1.CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide photo-anode, 2. polysulfide electrolyte and 3.CuS counter electrode.
FIG. 7 is a J-V test curve of quantum dot sensitized solar cells prepared in comparative examples 1 to 3; the curves labeled 1-3 in the figure correspond to comparative examples 1-3. The abscissa is the voltage (V) and the ordinate is the current density (mA cm)-2)。
Detailed Description
The present invention is further illustrated by, but not limited to, the following examples.
Example 1:
preparation of raw material zinc-tin hydrotalcite powder: 16.064g of Zn (NO) are taken3)2·6H2O, 2.104g SnCl4·5H2O、10.811g CO(NH2)2Dissolved in 400ml deionized water, and heated in an oil bath at 100 ℃ for 24 hours. And cleaning, filtering, drying and grinding the reaction product to obtain hydrotalcite-like powder with the molar ratio of zinc to tin of 9: 1.
Step A: the zinc-tin hydrotalcite powder is calcined in a muffle furnace at 500 ℃ for 1h to obtain the zinc-tin mixed metal oxide. As shown in fig. 1, the XRD pattern of the zinc-tin hydrotalcite-like compound shows the basic diffraction peaks (003), (006) and (009) of the hydrotalcite-like compound, and the sample has good crystallinity. The XRD pattern of the zinc-tin mixed metal oxide shows a strong diffraction peak consistent with the ZnO wurtzite structure, which shows that the zinc-tin hydrotalcite is completely reacted after being calcined to generate the mixed metal oxide with good crystallinity. Fig. 2 SEM images of (a) the zinc-tin hydrotalcite and (b) the zinc-tin mixed metal oxide show that both morphologies are dominated by sheet structures and that there is no significant change before and after calcination.
And B: and B, mixing 1g of zinc-tin mixed metal oxide, 4.4mL of terpineol and 10mL of ethyl cellulose in the step A, and stirring for 2-3 hours to obtain uniform slurry. The slurry was blade-coated on a fluorine-doped tin oxide conductive glass having a sheet resistance of 14. omega. to form a thickness of 25mm2A film of (2). And (3) placing the film in a muffle furnace, heating to 450 ℃ at the speed of 5 ℃/min, and keeping for 30min to obtain the zinc-tin mixed metal oxide nano porous film.
And C: 1.54g of Cd (NO)3)2·4H2Dissolving O in 50mL ethanol, collecting 1.2g Na2S·9H2O was dissolved in 50mL of an equal volume of a mixed solution of ethanol and deionized water. Placing the zinc-tin mixed metal oxide nano-porous film in the step B into Cd (NO)3)2Dissolving in the solution for 1min, taking out, washing with ethanol, drying, adding Na2And taking out the S solution after 1min, cleaning the S solution by using ethanol and drying the S solution, wherein the process is an adsorption cycle, and the adsorption cycle is totally 11 times to obtain the CdS quantum dot sensitized zinc-tin mixed metal oxide.
Step D: 0.79g of Se powder and 3.78g of Na are taken2SO3Dissolving in 100mL deionized water, heating at 90 deg.C for 7h to obtain Na2SeSO3An aqueous solution. Placing the CdS quantum dot sensitized zinc-tin mixed metal oxide obtained in the step C into a glass vessel, and adding Na with the same volume2SeSO3Aqueous solution, 0.1M Cd (NO)3)2And (3) immersing the aqueous solution and 0.2M sodium nitrilotriacetate aqueous solution in the film, and depositing for 4 hours at room temperature in a dark place to obtain the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide.
FIG. 2(c) SEM image of CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide and FIG. 2(d) element distribution diagram show that the main body morphology is unchanged after quantum dot sensitization, and the O, Zn, Sn, Cd, S and Se elements are uniformly distributed. As shown in fig. 3, the lattice fringes in the TEM image of the zinc-tin mixed metal oxide sensitized with CdS/CdSe quantum dots correspond to the (111) plane of CdSe, the (111) plane of CdS and the (100) plane of ZnO, and the XRD pattern of fig. 1 and the element distribution of fig. 2 show that the CdS and CdSe quantum dots are loaded on the zinc-tin mixed metal oxide. The light absorption of the zinc-tin mixed metal oxide with CdS quantum dot adsorption cycles of 11 times and CdSe quantum dot deposition for 4h is shown in curve 1 in fig. 4, which has good absorption in both the ultraviolet and visible range.
Step E: 2.4g of Na are taken2S·9H2O and 0.32g of sublimed sulfur are dissolved in 10mL of deionized water, and stirred for 2 hours at 50 ℃ to obtain the polysulfide electrolyte. Vertically placing fluorine-doped tin oxide conductive glass with sheet resistance of 7 omega in a glass vessel, adding a proper amount of 0.1M CuSO4、0.4M Na2S2O3And 0.4M CH4N2And (3) immersing the mixed aqueous solution of O in conductive glass, keeping away from light at 70 ℃ for 2.5h, taking out, cleaning and drying to obtain the CuS counter electrode.
Step F: and D, assembling the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide photo-anode obtained in the step D, the polysulfide electrolyte prepared in the step E and the CuS counter electrode into a battery with a sandwich structure by using a heat-sealing film. In FIG. 5, curve 1 is the J-V test result of CdS/CdSe quantum dot sensitized solar cell, and the short-circuit current density is 17.41mA cm-2The open-circuit voltage is 0.54V, the photoelectric conversion efficiency is 3.31%, and the photoelectric performance is good.
Example 2:
the procedure and process as described in example 1, except that: the CdS quantum dot adsorption cycle is 9 times, the CdSe quantum dot is deposited for 4h, the ultraviolet-visible light absorption (UV-vis) of the obtained CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide is shown as a curve 2 in a figure 4, and the light absorption intensity is slightly lower than that of an example 1 because the adsorption amount of the CdS quantum dot is less than that of the example 1. The J-V test result of the CdS/CdSe quantum dot sensitized solar cell is shown as a curve 2 in a graph 5, and the short-circuit current density is 16.68mA cm-2The open circuit voltage was 0.54V, and the photoelectric conversion efficiency was 3.24%.
Example 3:
the procedure and process as described in example 1, except that: adsorbing CdS quantum dot for 13 times, depositing CdSe quantum dot for 4h to obtain CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide with ultraviolet rayVisible light absorption is shown in curve 3 in fig. 4, and the light absorption intensity is higher than that of example 1 because the adsorption amount of the CdS quantum dots is greater than that of example 1. The J-V test result of the CdS/CdSe quantum dot sensitized solar cell is shown as curve 3 in FIG. 5, and the short-circuit current density is 15.79mA cm-2The open circuit voltage is 0.56V, and the photoelectric conversion efficiency is 2.92%.
Example 4:
the procedure and process as described in example 1, except that: the CdS quantum dot adsorption cycle is 11 times, the CdSe quantum dot is deposited for 3 hours, the ultraviolet-visible light absorption of the obtained CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide is shown as a curve 4 in a figure 4, and the light absorption intensity is low due to the short deposition time of the CdSe quantum dot. The J-V test result of the CdS/CdSe quantum dot sensitized solar cell is shown as curve 4 in FIG. 5, and the short-circuit current density is 15.38mA cm-2The open circuit voltage is 0.56V, and the photoelectric conversion efficiency is 2.96%.
Example 5:
the procedure and process as described in example 1, except that: the CdS quantum dot adsorption cycle is 11 times, the CdSe quantum dot is deposited for 5 hours, the ultraviolet-visible light absorption of the obtained CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide is shown as a curve 5 in a figure 4, and the light absorption intensity is improved because the CdSe quantum dot deposition time is longer. The J-V test result of the CdS/CdSe quantum dot sensitized solar cell is shown as curve 5 in FIG. 5, and the short-circuit current density is 17.57mA cm-2The open circuit voltage was 0.54V, and the photoelectric conversion efficiency was 3.14%.
Example 6:
the procedure and process as described in example 1, except that: the raw material zinc-tin hydrotalcite-like powder is prepared by weighing the raw materials according to the zinc-tin molar ratios of 7:1, 8:1, 10:1 and 11:1 respectively to prepare the hydrotalcite-like powder with the zinc-tin molar ratios of 7:1, 8:1, 10:1 and 11: 1. The prepared CdS/CdSe quantum dot sensitized solar cell is tested, and the performances are as the following table 1:
TABLE 1
Comparative example 1: single sensitization of CdS
As in example 1, except that: and D, omitting the step D, and assembling the CdS quantum dot sensitized zinc-tin mixed metal oxide in the step C as a photoanode, the polysulfide electrolyte in the step E and a CuS counter electrode into a sandwich-structured battery. The J-V test result of the CdS quantum dot sensitized solar cell is shown as curve 1 in FIG. 7, and the short-circuit current density is 6.56mA cm-2The open circuit voltage was 0.44V, and the photoelectric conversion efficiency was 0.82%. Because no CdSe quantum dots are deposited, the photo-generated charge is less, and the battery performance is lower than that of the embodiments 1-5.
Comparative example 2: hydrotalcite-like compound with zinc-tin molar ratio of 5:1
As in example 1, except that: 14.875g of Zn (NO) are taken3)2·6H2O and 3.506g of SnCl4·5H2O is used for preparing the zinc-tin hydrotalcite (zinc-tin molar ratio is 5: 1). The J-V test result of the CdS/CdSe quantum dot sensitized solar cell is shown as a curve 2 in a graph 7, and the short-circuit current density is 14.99mA cm-2The open circuit voltage is 0.57V, and the photoelectric conversion efficiency is 2.85%. The excessive tin content in the mixed metal oxide is not beneficial to quantum dot adsorption and charge transmission, and the short-circuit current density of the battery is low.
Comparative example 3: CdS adsorption cycle 5 times and CdSe deposition 6h
As in example 1, except that: and (3) carrying out CdS quantum dot adsorption cycle 5 times in the step C, and depositing CdSe for 6 hours in the step D. The J-V test result of the CdS/CdSe quantum dot sensitized solar cell is shown as curve 3 in FIG. 7, and the short-circuit current density is 13.13mA cm-2The open circuit voltage is 0.56V, and the photoelectric conversion efficiency is 2.12%. Because fewer CdS quantum dots and more CdSe quantum dots are used, the recombination of photo-generated charges is intensified, and the short-circuit current density is reduced.
Claims (10)
1. A CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite comprises conductive glass, a semiconductor film and CdS and CdSe quantum dots sequentially loaded on the semiconductor film; wherein the content of the first and second substances,
the semiconductor film is a nano-porous semiconductor film of mixed metal oxide formed by calcining zinc-tin hydrotalcite, and the molar ratio of zinc to tin in the zinc-tin hydrotalcite is 7-11: 1;
the CdS and CdSe quantum dots sequentially loaded on the semiconductor film are obtained by firstly carrying out CdS quantum dot adsorption circulation on the semiconductor film for 8-14 times and then carrying out CdSe quantum dot deposition for one time.
2. The CdS/CdSe quantum dot sensitized solar cell photoanode as defined in claim 1, wherein CdS and CdSe quantum dots sequentially loaded on the semiconductor thin film are prepared by performing CdS quantum dot adsorption cycle on the semiconductor thin film for 9-13 times, and then performing CdSe quantum dot deposition once; the preferable deposition time of the CdSe quantum dots is 3-5 hours.
3. The CdS/CdSe quantum dot sensitized solar cell photoanode according to claim 1, wherein the CdS quantum dot adsorption is to immerse a semiconductor thin film in a Cd-containing cation solution, take out, clean, dry and then immerse in an S-containing anion solution, in any order; preferably, the cation solution is 0.05-0.3M Cd (NO)3)2The S anion-containing solution is 0.05-0.3M of Na2S ethanol water solution; more preferably, the conductive glass is fluorine-doped tin oxide conductive glass with the sheet resistance of 10-15 omega.
4. The method for preparing the CdS/CdSe quantum dot sensitized solar cell photo-anode based on zinc-tin hydrotalcite like compound according to any one of claims 1 to 3, comprising the steps of:
(1) calcining zinc-tin hydrotalcite powder at 400-700 ℃ to obtain a zinc-tin mixed metal oxide;
(2) preparing the prepared zinc-tin mixed metal oxide into slurry by using a solvent and an auxiliary agent, coating the slurry on conductive glass to form a film, then placing the film in a muffle furnace, heating to 400-500 ℃, and keeping the temperature for 20-40 min to obtain a nano porous semiconductor film of the zinc-tin mixed metal oxide;
(3) placing the zinc-tin mixed metal oxide nano-porous film in Cd (NO)3)2Adding the mixture into the solution for 0.5-2 min, taking out, washing with ethanol, drying, and adding Na2Taking out the S solution after 0.5-2 min, cleaning with ethanol and drying, wherein the above processes are a cycle, and the cycle is totally 8-14 times to obtain the CdS quantum dot sensitized zinc-tin mixed metal oxide;
(4) immersing the CdS quantum dot sensitized zinc-tin mixed metal oxide prepared in the step (3) in Na with the same volume2SeSO3Aqueous solution, Cd (NO)3)2And depositing the mixed solution consisting of the aqueous solution and the sodium nitrilotriacetate aqueous solution at room temperature in a dark place for 3-5 hours to obtain the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide, namely the CdS/CdSe quantum dot sensitized solar cell photo-anode.
5. The method of preparing the CdS/CdSe quantum dot sensitized solar cell photoanode according to claim 4, wherein the step (1) comprises one or more of the following conditions:
a. the size of the zinc-tin mixed metal oxide is 100-500 nm;
b. the zinc-tin hydrotalcite powder is calcined in a muffle furnace;
c. the zinc-tin hydrotalcite powder is prepared by the following method: taking Zn (NO) according to the molar ratio of zinc to tin of 7-11: 13)2·6H2O、SnCl4·5H2O, and an appropriate amount of CO (NH)2)2Dissolving in deionized water, heating in an oil bath at 95-100 ℃ for 20-26 h, and cleaning, filtering, drying and grinding reaction products to obtain the zinc-tin hydrotalcite powder.
6. The method of preparing the CdS/CdSe quantum dot sensitized solar cell photo-anode according to claim 4, wherein the step (2) includes one or more of the following conditions:
a. the solvent is terpineol or organic silicone oil;
b. the auxiliary agent is ethyl cellulose or butyl cellulose;
c. the mass volume ratio of the zinc-tin mixed metal oxide to the solvent is 1: 4-5, and the unit g: mL;
d. the mass volume ratio of the zinc-tin mixed metal oxide to the auxiliary agent is 1: 9-12, and the unit g: mL;
e. and the temperature is increased at the speed of 3-6 ℃/min.
7. A CdS/CdSe quantum dot sensitized solar cell based on zinc-tin hydrotalcite is characterized in that a sandwich structure is formed by a photo-anode, an electrolyte and a counter electrode; wherein the content of the first and second substances,
the photo-anode is the CdS/CdSe quantum dot sensitized solar cell photo-anode of any one of claims 1-3;
the electrolyte is polysulfide electrolyte composed of Na2S·9H2Dissolving O and sublimed sulfur in deionized water to obtain the product;
the counter electrode is a CuS counter electrode.
8. The method for preparing CdS/CdSe quantum dot sensitized solar cell based on zinc-tin hydrotalcite like compound according to claim 7 comprises the following steps:
1) a method of preparing a CdS/CdSe quantum dot sensitized solar cell photoanode as defined in any one of claims 1-3;
2) preparation of polysulfide electrolyte
Taking Na according to the molar ratio of 1-3: 12S·9H2Dissolving O and sublimed sulfur in deionized water to make Na2S·9H2Stirring at 45-55 ℃ with the molar concentration of O being 1-3 mol/L to obtain polysulfide electrolyte;
3) preparation of CuS counter electrode
Vertically placing fluorine-doped tin oxide conductive glass in a container, and adding a solution containing 0.05-0.2M of CuSO4、0.2～0.8M Na2S2O3And 0.2 to 0.8M CH4N2O, enabling the mixed water solution to submerge the conductive glass, keeping away from light at the temperature of 60-80 ℃ for 2-3 hours, taking out, cleaning and drying to obtain a CuS counter electrode;
4) assembly
And sequentially assembling the CdS/CdSe quantum dot sensitized zinc-tin mixed metal oxide photo-anode, the polysulfide electrolyte and the CuS counter electrode into a sandwich-structured battery by using a heat-sealing film.
9. The method of preparing a zinc tin hydrotalcite-based CdS/CdSe quantum dot sensitized solar cell according to claim 8, characterized in that it comprises one or more of the following conditions:
a. in the step 2), the sulfur is sublimed sulfur;
b. in step 2), equimolar amounts of Na are added2S·9H2Dissolving O and sulfur in deionized water to prepare 1M Na2S and 1M aqueous solution of sublimed sulphur;
c. in the step 3), the mixed aqueous solution contains 0.08-0.1M CuSO4、0.4～0.5M Na2S2O3And 0.4 to 0.5M CH4N2O；
d. And step 3), the conductive glass is fluorine-doped tin oxide conductive glass with the square resistance of 5-8 omega.
10. The use of the CdS/CdSe quantum dot sensitized solar cell as defined in claim 7 in solar power generation on the outer surface of buildings, power supplies of low-power electronic devices or flexible power generation products collocated with textiles.
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