CN113851586B - Composite film, preparation method thereof and solar cell comprising composite film - Google Patents
Composite film, preparation method thereof and solar cell comprising composite film Download PDFInfo
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Abstract
The invention relates to a composite film, a preparation method thereof and a solar cell comprising the composite film. The composite film comprises Zn 2 SnO 4 、ZnSnO 3 ZnO and SnO 2 Four components and has a work function of 3.53eV as determined by uv electron spectroscopy. The composite film is used as a cathode modification layer of the solar cell, so that the energy conversion efficiency of the solar cell is improved.
Description
Technical Field
The invention relates to the field of preparation of photovoltaic materials and devices, in particular to a composite film, a preparation method thereof and a solar cell comprising the composite film.
Background
Energy is an important material basis on which human society relies to survive and develop. Traditional fossil energy faces the crisis of exhaustion on one hand, and causes huge damage to the environment on the other hand. The search for clean, new renewable energy sources has become an urgent need in human society. Solar energy belongs to green, environment-friendly and pollution-free new energy, has the characteristics of inexhaustibility and inexhaustibility compared with the human society, and is increasingly concerned and valued by people. The solar cell has wide raw material sources and simple preparation process, can be prepared into a large-area membrane by industrial methods such as spin coating, spraying, squeegee printing and the like, and has wide application prospect. For the industrialization of solar cells, there is a need to improve the energy conversion efficiency and stability.
Disclosure of Invention
The invention aims to provide a composite film, a preparation method thereof and a solar cell comprising the composite film, and the composite film can be used for improving the energy conversion efficiency and stability of a polymer solar cell.
In one aspect, the present invention provides a composite film comprising Zn 2 SnO 4 、ZnSnO 3 ZnO and SnO 2 Four components and has a work function of 3.53eV as determined by uv photoelectron spectroscopy.
In one example, the thickness of the composite film is 10 to 40nm, preferably 30nm.
The composite film is used as a cathode modification layer of the solar cell, so that the energy conversion efficiency of the solar cell reaches 12.50%.
In another aspect, the present invention provides a method for preparing a composite film comprising
Mixing a solution A containing zinc acetate dihydrate and a solution B containing tin tetrachloride pentahydrate to form a stable colloidal solution C, wherein the molar ratio of the zinc acetate dihydrate to the tin tetrachloride pentahydrate is 1.5; and
and spin-coating the colloidal solution C on a substrate, and annealing at 180 ℃ to form a compact composite film.
In one example, the solution a further contains a chelating agent.
In one example, the chelating agent is ethanolamine, and the molar ratio of the zinc acetate dihydrate to the ethanolamine is 1.
In one example, the solution a further contains an organic solvent, and the organic solvent is ethylene glycol monomethyl ether.
In one example, the solution B further contains water.
In another aspect, the invention provides a solar cell comprising the composite film as a cathode modification layer.
In one example, the solar cell of the present invention includes a substrate, a cathode, the cathode modification layer, an active layer, an anode modification layer, and an anode stacked in this order from bottom to top.
Compared with ZnO thin film and SnO in the prior art 2 Compared with the film, the work function of the composite film is obviously reduced. For the solar cell using the composite film as the cathode modification layer, the lower work function of the composite film leads the energy level potential barrier of electron transportation at the cathode to be reduced, thereby being beneficial to the transmission of the electron at the cathode modification layer and the collection of the electron by the cathode, improving the open-circuit voltage and the short-circuit current density of the solar cell and obviously improving the performance of the solar cell. In addition, the solar power of the inventionThe cell has more excellent stability.
Drawings
Fig. 1 shows the XRD diffractogram of the composite thin film of the present invention.
Fig. 2 shows a uv electron spectroscopy (UPS) diagram of a composite film according to the present invention.
Fig. 3 is a schematic structural view of a solar cell using the composite thin film according to the present invention as a cathode modification layer.
Fig. 4 shows a current density-voltage characteristic graph of the solar cells prepared according to comparative examples 1-2 and example 3.
Fig. 5 shows stability profiles of solar cells prepared according to comparative examples 1-2 and example 3.
Detailed Description
For a better understanding of the present invention, reference is made to the following detailed description taken in conjunction with the accompanying drawings and examples. It should be understood that the embodiments described herein are for the purpose of illustrating the invention and are not intended to limit the scope of the invention.
In the prior art, the cathode modification layer of the solar cell is a ZnO film or SnO 2 Thin films, znO or SnO 2 Has a high work function, znO film or SnO 2 The solar cell using the thin film as the cathode modification layer has low energy conversion efficiency, thereby limiting the development and utilization of the solar cell.
The invention aims to provide a composite film with a remarkably reduced work function, and the composite film is used as a cathode modification layer to improve the energy conversion efficiency and stability of a solar cell.
In one embodiment, the present invention provides a composite film comprising: zn 2 SnO 4 、ZnSnO 3 ZnO and SnO 2 Four components. In one example, the thickness of the composite film is 10 to 40nm, preferably 30nm.
The inventors found that the work function of the composite film of the present invention is significantly reduced. For the solar cell using the composite film as the cathode modification layer, the lower work function of the composite film leads the energy level potential barrier of the electron transported at the cathode to be reduced, thereby being beneficial to the transmission of the electron at the cathode modification layer and the collection of the electron by the cathode, improving the open-circuit voltage and the short-circuit current density of the solar cell and obviously improving the performance of the solar cell.
In another embodiment, the present invention provides a method for preparing a composite film, the method comprising the steps of:
mixing a solution A dissolved with zinc acetate dihydrate and a solution B dissolved with tin tetrachloride pentahydrate to form a stable colloidal solution C, wherein the molar ratio of the zinc acetate dihydrate to the tin tetrachloride pentahydrate is 1.5:1-2.5:1; and
and spin-coating the colloidal solution C on a substrate, and annealing at 180 ℃ to form a compact composite film.
In one example, the solution a further contains a chelating agent.
In one example, the chelating agent is ethanolamine and the molar ratio of the zinc acetate dihydrate to the ethanolamine is 1:1.
In one example, the solution a further contains an organic solvent, and the organic solvent is ethylene glycol monomethyl ether.
In one example, the solution B further contains water.
In one embodiment, zinc acetate dihydrate Zn (Ac) 2 ·2H 2 O (i.e. Zn (CH)) 3 COOH) 2 ·2H 2 O) is dissolved in an organic solvent ethylene glycol monomethyl ether, and the zinc acetate dihydrate undergoes the following hydrolysis reaction in the process:
due to chelating agent ethanolamine (HOCH) 2 CH 2 NH 2 ) So that the precipitate Zn (OH) 2 A polycondensation reaction occurs to produce:
H-(O-Zn-O-Zn-O)n-H
tin tetrachloride pentahydrate (SnCl) 4 ·5H 2 O) is dissolved in water, during which the following reaction takes place:
when the solution A and the solution B are mixed, because the ethanolamine simultaneously acts as a stabilizer and a chelating agent, the hydrolysis can be promoted and the chelating effect is achieved, and after the solution A and the solution B are fully mixed, a stable colloidal solution is generated.
The stable colloidal solution mainly contains:
in one embodiment, the resulting colloidal solution has a concentration of 0.25mol/ml.
During the annealing process, organic matters in the organic polymer taking H- (O-Zn-O-Sn-O-Zn-O) -H as an organism are decomposed to form compact Zn-containing polymers 2 SnO 4 、ZnSnO 3 ZnO and SnO 2 The composite film of (1).
The method for preparing the composite film is simple to operate and does not need high-temperature treatment. The composite film prepared by the method has lower work function. The solar cell using the composite film as the cathode modification layer has obviously improved photovoltaic performance and stability.
In another aspect, the invention provides a solar cell comprising the composite film as a cathode modification layer.
In one example, the solar cell of the present invention includes a substrate, a cathode, the cathode modification layer, an active layer, an anode modification layer, and an anode stacked in this order from bottom to top.
In one example, the substrate is a glass substrate, the cathode layer is Indium Tin Oxide (ITO); the thickness of the cathode modification layer is 10-40 nm, and preferably 30nm.
The active layer comprises (1) PTB7 or PM7 (also known as PBDB-T-C1, poly [ (2, 6- (4, 8-bis (5- (2-ethylhexyl-3-chloro) thiophen-2-yl) -benzo [1,2-b:4,5-b']Bithiophene)) -random- (5, 5- (1 ',3' -di-2-thienyl-5 ',7' -bis (2-ethylhexyl) benzo [1',2' -c:4',5' -c ']Dithiophene-4, 8-dione), cas:2239295-71-5])、(2)PC 71 BM or ITIC-4F (3, 9-bis (2-methylene- ((3- (1, 1-dicyanomethylene) -6, 7-difluoro) -indanone)) -5, 11, 11-tetrakis (4-hexylphenyl) -dithieno [2,3-d:2',3' -d ']-s-benzodiindeno [1,2-b:5,6-b']Dithiophene, cas: 2097998-59-7), and (3) additives. The thickness of the active layer is 80 to 120nm, preferably 100nm.
The anode modification layer is MoO 3 The thickness of the anode modification layer is 5-15 nm, preferably 10nm.
The anode layer is Ag, and the thickness of the anode layer is 80-100 nm.
A method for preparing a solar cell as described above, comprising the steps of:
1) Providing a substrate;
2) Preparing a cathode layer on the substrate;
3) Preparing a cathode modification layer on the cathode layer;
4) Preparing an active layer on the cathode modification layer;
5) Preparing an anode modification layer on the active layer;
6) And preparing an anode layer on the anode modification layer.
In one example, the active layer is formed by spin coating a mass/volume (w/v) of 12.5mg/ml to 10mg/ml of PM7: prepared from an ITIC-4F solution; the solution also preferably contains ortho-xylene. The active layer solution is doped with 0.5 to 3 volume percent of additive. Preferably, the active layer solution is doped with 1% by volume of an additive.
With ZnO thin film and SnO in the prior art 2 Compared with the film, the work function of the composite film is obviously reduced. For the solar cell using the composite film as the cathode modification layer, the lower work function of the composite film leads the energy level potential barrier of the electron transported at the cathode to be reduced, thereby being beneficial to the transmission of the electron at the cathode modification layer and the collection of the electron by the cathode, improving the open-circuit voltage and the short-circuit current density of the solar cell and obviously improving the performance of the solar cell. The solar cell using the composite film of the invention as a cathode modification layer has the performance of 93 percent of the original performance after 6 months of attenuation test. Stability tests show that the solar cell provided by the invention has more excellent stability.
Examples
The experimental methods used in the present invention are all conventional methods unless otherwise specified.
The materials, reagents and the like used in the present invention are commercially available unless otherwise specified.
The experimental reagent and the instrument used in the invention are as follows:
o-xylene, 1-8 dichlorooctane (DClO), ethanolamine, zinc acetate dihydrate, ethylene glycol methyl ether, available from carbofuran technologies, inc.;
tin tetrachloride pentahydrate was purchased from Sigma-Aldrich;
PM7 (batch: YY15156 CH), ITIC-4F (batch: DW 3262B) was purchased from 1-Materials, canada;
high purity silver pellets (purity > 99.999%) for plating electrodes were purchased from chenopodium corporation.
The ITO glass substrate used in the invention is purchased from Shenzhen south China Xiang City science and technology Limited, and the sheet resistance is 15 omega/\ 9633.
The spin coater was purchased from a KW-4A model desk spin coater designed and manufactured by the microelectronics institute of the Chinese academy of sciences.
Photovoltaic of solar cellPerformance parameters were measured at 100mW/cm using a Keithley 2400 digital Source Meter 2 The current density-voltage characteristic curve of the standard simulated sunlight (AM 1.5G) is measured and calculated.
The thicknesses of the cathode modification layer and the active layer were measured by a Dektak XT type probe profilometer of Bruker, USA.
The characterization of the UV-photoelectron spectroscopy of the composite film of the present invention was measured by a multifunctional photoelectron spectrometer (Shimadzu, japan/Kratos).
Characterization of the X-ray diffraction (XRD) spectra of the composite films was obtained by X-ray diffractometer (Bruker D8 Advance, USA) measurements.
EXAMPLE 1 preparation of films
1. Preparation of the solution
1.1 preparation of solution A
164.61mg of zinc acetate dihydrate (Zn (Ac) 2 ·2H 2 O) and 45.81mg of Ethanolamine (C) 2 H 7 NO) (molar ratio 1). In the resulting solution A, ethanolamine concentration was 0.75mol/ml, zn (Ac) 2 ·2H 2 The solubility of O was 0.75mol/ml.
1.2 preparation of solution B
262.5mg of tin tetrachloride pentahydrate (SnCl) were taken 4 ·5H 2 O) to 1ml of water, stirring until dissolved to form a solution B, and adding SnCl to the resulting solution B 4 ·5H 2 The O concentration was 0.75mol/ml.
1.3 preparation of colloidal solution C
500. Mu.l of the solution A was added to 250. Mu.l of the solution B, and stirred at 60 ℃ for 12 hours until dissolved, to form a stable colloidal solution, thereby obtaining a colloidal solution C.
After the preparation of the above solution a, solution B and colloidal solution C was completed, the solution a, solution B and colloidal solution C were filtered using an organic filter with a pore size of 0.22 μm, respectively, and the filtrates were collected for subsequent use.
2. Preparation of the film
2.1 preparation of ZnO films
Solution a was spin-coated onto an ITO glass substrate at 3500rpm/min and annealed at 200 ℃ for 60min to form a dense ZnO thin film (comparative example 1).
2.2SnO 2 Preparation of films
Spin-coating the solution B on an ITO glass substrate at 3500rpm/min, and annealing at 150 deg.C for 30min to form dense SnO 2 Film (comparative example 2).
2.3 preparation of the composite film of the invention
And spin-coating the colloidal solution C on an ITO glass substrate at the rotating speed of 3500rpm/min, and annealing at 180 ℃ for 30min to form a compact composite film.
EXAMPLE 2 testing of the films
1.X-ray diffraction Pattern determination
The composite film of the present invention obtained in example 1 was analyzed by an X-ray diffractometer model D8 Advances of Bruker, and the results are shown in FIG. 1.
As shown in FIG. 1, the composite film of the present invention contains Zn 2 SnO 4 、ZnSnO 3 ZnO and SnO 2 Four components.
2. Ultraviolet Photoelectron Spectroscopy (UPS) test
Ultraviolet photoelectron spectroscopy is an effective technique for measuring the work function of a substance.
ZnO thin film and SnO prepared in example 1 2 The films and the composite films of the present invention were subjected to UPS test, and the results are shown in table 1 below and fig. 2.
TABLE 1
As can be seen from Table 1, the work function of the ZnO film was 4.57eV 2 The work function of the film was 4.04eV, whereas the work function of the composite film of the present invention was 3.53eV. The results show that the work function of the composite film of the present invention is significantly reduced.
Example 3 preparation of a solar cell of the invention
1. Preparation of active layer solution
Taking o-xylene as a solvent, mixing PM7 with the mass/volume (w/v) of 12.5mg/ml to 10 mg/ml: the ITIC-4F was dissolved in an o-xylene solution, and 1% by volume of DClO was added thereto, followed by stirring at 60 ℃ for 6 hours to obtain an active layer solution.
2. Preparation of cathode modification layer
The transparent conductive glass containing ITO is placed in a cleaning solution for ultrasonic treatment for 1 hour, then the ITO glass is sequentially placed in deionized water and alcohol (the concentration is 99.5 percent), and ultrasonic treatment is sequentially carried out for 30 minutes. And carrying out ultraviolet ozone treatment on the ITO cathode layer for 8min to obtain the substrate containing the ITO cathode. Preparing the colloidal solution C as described in example 1, spin-coating the filtered colloidal solution C onto an ITO glass substrate at 3500rpm/min using a spin coater, and annealing at 180 deg.C for 30min to form a dense Zn-containing film 2 SnO 4 、ZnSnO 3 ZnO and SnO 2 The composite nano film of the component (A) has a film thickness of 30nm.
3. Preparation of solar cell
And spin-coating the active layer solution on the composite nano film by using a spin coater to prepare the active layer, wherein the rotation speed of the spin coater is 1000rpm, and the spin-coating time is 50s. Then transferring the prepared active layer film to a vacuum coating cavity for evaporating an anode modification layer MoO 3 And Ag electrode, the vacuum degree in the cavity is maintained at 2X 10 -4 Pa, real-time monitoring of evaporation rate and film thickness by quartz crystal oscillator, moO 3 Has an evaporation rate of
The thickness is 8nm; the evaporation rate of Ag is
The thickness was 100nm. And after the film coating is finished, obtaining the solar cell. The structure of the prepared solar cell device is shown in fig. 3.
Comparative example 1 preparation of solar cell of comparative example 1
Preparation of solar cell with ZnO film as cathode modification layer
A solar cell in which a ZnO thin film was used as a cathode modification layer was prepared in substantially the same manner as in example 3. The same procedure as in example 3 was repeated except that the method for preparing the cathode modification layer was different.
Preparing a cathode modification layer: solution A was prepared as described in example 1, then spin coated onto an ITO glass substrate at 3500rpm/min and annealed at 200 ℃ for 60min to form a dense ZnO film.
Comparative example 2 preparation of solar cell of comparative example 2
2.SnO 2 Preparation of solar cell with thin film as cathode modification layer
SnO was prepared by substantially the same procedure as in example 3 2 The film is used as a solar cell of the cathode modification layer. The operation was the same as the solar energy production method described in example 3, except that the method for producing the cathode modification layer was different.
Preparing a cathode modification layer: solution B was prepared as described in example 1, then spin-coated onto an ITO glass substrate at 3500rpm/min and annealed at 150 ℃ for 30min to form dense SnO 2 A film.
Example 4 Performance testing of solar cells
Using a Keithley 4200 digital source table at 100mW/cm 2 The current density-voltage characteristic curves of the solar cells prepared in example 3, comparative examples 1 and 2 were measured under standard simulated sunlight (AM 1.5G), and the photovoltaic performance parameters of the solar cells were calculated from the current density-voltage characteristic curves: open circuit voltage (U) oc ) Short circuit current density (J) sc ) Fill Factor (FF), and energy conversion efficiency (PCE).
The open-circuit voltage refers to the voltage generated by the device after illumination when no current loop exists;
the short-circuit current density refers to the current density which can be generated when the illuminated device forms a loop when the applied voltage is zero;
the fill factor refers to the maximum output power (U) of the battery m J m ) And the ratio of the product of the open circuit voltage and the short circuit current density is as follows:
energy conversion efficiency (PCE) refers to the maximum output power P m And irradiation power P in In a ratio of
In the formula, J SC Is short circuit current density in mA/cm 2 ；P in Is the irradiation power, with the unit of mW/cm 2 。
The results of measuring the performance of the solar cells prepared in example 3 and comparative examples 1 and 2 are shown in table 2. The current density-voltage characteristic curves of the solar cells prepared in example 3 and comparative examples 1 and 2 are shown in fig. 4.
TABLE 2
As can be seen from the test results of Table 2 and FIG. 4, the short-circuit current density of the solar cell prepared using the ZnO thin film as the cathode modification layer was 17.96mA/cm 2 The open-circuit voltage is 0.86V, the fill factor is 64%, and the energy conversion efficiency is 9.82%; with SnO 2 The solar cell prepared by using the film as a cathode modification layer has the energy conversion efficiency of 10.91 percent and the short-circuit current density of 17.96mA/cm 2 The open circuit voltage was 0.86V, and the fill factor was 64%. The solar cell using the composite film of the present invention as a cathode modification layer is shortThe current density, open-circuit voltage and fill factor of the circuit are obviously improved, and the energy conversion efficiency is obviously improved to 12.50 percent.
Example 5 stability testing of solar cells
Solar cell (comparative example 1) using ZnO thin film as cathode modification layer, snO 2 The solar cell (comparative example 2) using the thin film as the cathode modification layer and the solar cell (example 3) using the composite thin film of the present invention as the cathode modification layer were placed in an air atmosphere with humidity of 30-40% and temperature of 25 ℃, the photovoltaic performance parameters of all the solar cells were periodically tested, and the subsequent test results were normalized with reference to the energy conversion efficiency (PCE) obtained by the first test of each solar cell, to obtain the stability data of each solar cell, with the results shown in fig. 5.
After 6 months of attenuation, the performance of the solar cell with the ZnO film as the cathode modification layer is attenuated to 80 percent, and SnO 2 The performance decay of the solar cell with the film as the cathode modification layer is 88%, while the performance of the solar cell with the composite film of the invention as the cathode modification layer is 93%. Stability tests show that the solar cell with the composite film as the cathode modification layer has more excellent stability.
Claims (2)
1. A method for preparing a composite film comprising
Mixing a solution A containing zinc acetate dihydrate and a solution B containing tin tetrachloride pentahydrate to form a stable colloidal solution C, wherein the molar ratio of the zinc acetate dihydrate to the tin tetrachloride pentahydrate is 1.5; and
spin-coating the colloidal solution C on a substrate, and annealing at 180 ℃ to form a compact composite film
The solution A also contains a chelating agent;
the chelating agent is ethanolamine, and the molar ratio of the zinc acetate dihydrate to the ethanolamine is 1;
the solution A also contains an organic solvent, and the organic solvent is ethylene glycol monomethyl ether.
2. The method of claim 1, wherein solution B further comprises water.
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| CN104241529A (en) * | 2013-06-17 | 2014-12-24 | 宁波大学 | Laminated organic solar battery and manufacturing method thereof |
| CN108546936A (en) * | 2018-05-09 | 2018-09-18 | 武汉理工大学 | A kind of method of low temperature preparation high-performance ZnO base transparent conductive oxide film |
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| CN108546936A (en) * | 2018-05-09 | 2018-09-18 | 武汉理工大学 | A kind of method of low temperature preparation high-performance ZnO base transparent conductive oxide film |
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