CN112490363B - Preparation method of perovskite solar cell based on magnetron sputtering zinc oxide/tin dioxide double electron transmission layer - Google Patents
Preparation method of perovskite solar cell based on magnetron sputtering zinc oxide/tin dioxide double electron transmission layer Download PDFInfo
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Abstract
The invention discloses a perovskite solar cell based on magnetron sputtering zinc oxide/tin dioxide double electron transmission layers, wherein the perovskite solar cell with double electron transmission layers is formed by taking magnetron sputtering zinc oxide as an electron transmission layer and spin-coating tin dioxide, so that the mobility of the electron transmission layer is improved, the compactness of a film is improved, the carrier transmission is improved, and the photoelectric conversion efficiency and the stability of a device are improved. According to the invention, the zinc oxide and tin dioxide electron transport layer can be prepared at low temperature, and the stable high-performance perovskite solar cell can be obtained.
Description
Technical Field
The invention relates to a solar cell preparation technology, in particular to a preparation method of a perovskite solar cell based on magnetron sputtering zinc oxide/tin dioxide double electron transmission layers, and belongs to the technical field of solar cells.
Background
With the increasing urgency of environmental pollution and energy exhaustion, the search for a renewable green energy source to replace the traditional fossil energy source has become a common concern for all people. The solar cell directly converts solar energy into electric energy, has the advantages of environmental protection, safety, reliability, long service life and the like, and has become a research hotspot at home and abroad. Currently, the market of silicon-based solar cells is the highest, but the long-term development of the silicon-based solar cells is restricted due to high cost, complex process and the like. Therefore, people gradually turn their attention to novel photovoltaic materials with low cost, low energy consumption and rich raw materials.
Compared with the traditional silicon-based solar cell, the perovskite solar cell has attracted extensive attention as a next-generation novel photovoltaic device, and the perovskite solar cell structurally comprises a transparent conductive substrate, an electron transmission layer, a perovskite absorption layer, a hole transmission layer and a metal electrode. Due to the excellent light absorption performance, high carrier mobility, long carrier life and diffusion length, the perovskite material is more suitable for solar cell devices. The main functions of the electron transport material in the battery are blocking hole transport and balancing electron hole transport distance, which has important influence on the performance of the battery.
Disclosure of Invention
The invention provides a preparation method of a perovskite solar cell based on magnetron sputtering zinc oxide/tin dioxide double electron transport layers. According to the invention, magnetron sputtering zinc oxide is used as an electron transport layer, and tin dioxide is spin-coated to form the perovskite solar cell with double electron transport layers, so that the mobility of the electron transport layer is improved, the compactness of a film is improved, the carrier transport is improved, and the photoelectric conversion efficiency and stability of a device are improved.
The invention relates to a perovskite solar cell based on magnetron sputtering zinc oxide/tin dioxide double electron transmission layers, which is prepared by a method comprising the following steps:
step 1: fixing a zinc oxide target in a cavity, fixing FTO conductive glass above the target, closing the cavity, sputtering zinc oxide by using a bipolar pulse power supply, adjusting oxygen to 6.0-8.0sccm and argon to 45-55sccm at a pressure ratio of 1-3Pa for 1-2 minutes, and taking out after sputtering is finished;
step 2: spin-coating the film obtained in the step 1 with a tin dioxide solution at 3000rmp/30s, and then annealing in the air at 150-160 ℃ for 30 minutes to obtain a layer of tin dioxide film on zinc oxide;
and step 3: and (3) spin-coating a perovskite light absorption layer and a hole transport layer on the tin dioxide-zinc oxide double electron transport layer obtained in the step (2), and finally evaporating a silver electrode, so that the perovskite solar cell based on the tin dioxide and magnetron sputtering zinc oxide double electron transport layer is obtained.
In the step 1, the sputtering distance between the target and the FTO conductive glass is controlled to be 4-6cm.
In step 2, the tin dioxide solution is a tin dioxide hydrosol (15%, available from febazierdinaceae) and is diluted with water in a volume ratio of 1.
In step 3, the perovskite light-absorbing layer is prepared by a method comprising the following steps: 0.461g of lead iodide (PbI) was taken 2 ) And 0.159g of methyl amine iodide (CH) 3 NH 3 I) Putting the medicine into a brown bottle, respectively dropwise adding 635ul of Dimethylformamide (DMF) and 72ul of dimethyl sulfoxide (DMSO) into the bottle by using a pipette, adding a rotor, magnetically stirring for 1 hour, and filtering to obtain a perovskite solution; and spin-coating the perovskite solution on a spin coater at the speed of 4000rmp/25s, dripping an ethyl acetate anti-solvent at the 5 th s, and finally annealing at 70 ℃ for 20min to obtain the perovskite absorption layer. All the above operations are carried out in a glove box.
In step 3, the hole transport layer is prepared by a method comprising the steps of: dissolving 72.3mg of Spiro-OMeTAD drug in 1ml of chlorobenzene solution, sequentially dropwise adding 29ul of 4-tert-butylpyridine (4-TBP) and 18ul of Li-TFSI, then adding a rotor, magnetically stirring for 40min, and filtering to obtain a Spiro-OMeTAD solution; the void layer was obtained by spin-coating a Spiro-OMeTAD solution at a speed of 3000rmp/30s on a spin coater. The above operation was also performed in a glove box.
Compared with the most common titanium oxide electron transport material at present, zinc oxide has similar energy level position as titanium oxide, higher electron transport rate and various preparation methods. The invention adopts a magnetron sputtering method to prepare a compact zinc oxide film and uses tin dioxide for modification, the annealing temperature only needs 150 ℃, the energy consumption can be greatly reduced, the flexible application is not influenced, the performance of the battery is greatly improved, and the stability of the battery is improved.
Compared with the prior art, the invention has the beneficial effects that:
the perovskite solar cell based on the magnetron sputtering zinc oxide/tin dioxide double electron transmission layer has the following advantages:
(1) The tin dioxide is added, so that direct contact between zinc oxide and perovskite is avoided to a certain extent, the thermal stability is improved, the decomposition of the perovskite is inhibited, and a high-quality perovskite absorption layer is formed;
(2) The addition of the tin dioxide fills oxygen vacancy, greatly reduces charge recombination of a perovskite/ZnO interface, and provides a more appropriate energy level and higher carrier mobility;
(3) The open-circuit voltage of the cell is improved to a certain extent, so that the photoelectric conversion efficiency is improved;
(4) The method has the advantages of low preparation temperature and simple preparation method, so that the method can be used for preparing the flexible substrate, thereby obtaining high photoelectric conversion efficiency and being suitable for large-scale production.
Drawings
Fig. 1 is a schematic structural diagram of a perovskite solar cell based on a magnetron sputtering zinc oxide/tin dioxide double electron transport layer. Wherein 1 is conductive glass (FTO), 2 is magnetron sputtering zinc oxide, 3 is stannic oxide, 4 is perovskite light absorption layer, 5 is hole transport layer, and 6 is silver electrode.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the surface of a magnetron sputtered zinc oxide/tin dioxide dual electron transport layer. As can be seen from FIG. 2, the magnetron sputtering zinc oxide/tin dioxide double electron transport layer has a compact and smooth surface, which is beneficial to the deposition of a perovskite layer.
FIG. 3 is a Scanning Electron Microscope (SEM) photograph of the surface of a perovskite on a magnetron sputtered zinc oxide/tin dioxide dual electron transport layer. As can be seen from FIG. 3, the perovskite thin film deposited on the magnetron sputtering zinc oxide/tin dioxide double electron transport layer is more compact and uniform.
FIG. 4 is a Scanning Electron Microscope (SEM) photograph of a cross section of a magnetron sputtered zinc oxide/tin dioxide dual electron transport layer. As can be seen in fig. 4, the zinc oxide is deposited relatively uniformly over the FTO and a thin film of tin dioxide is deposited over the zinc oxide.
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of a cross section of a perovskite on a magnetron sputtered zinc oxide/tin dioxide dual electron transport layer. As can be seen from fig. 5, a perovskite thin film is deposited on the magnetron sputtered zinc oxide/tin dioxide dual electron transport layer.
FIG. 6 is an XRD spectrum of perovskite on a magnetron sputtered zinc oxide/tin dioxide dual electron transport layer. As can be seen from FIG. 6, the film deposited on the magnetron sputtering zinc oxide/tin dioxide double electron transport layer satisfies the corresponding diffraction peaks of the perovskite film, and the deposited film is proved to be the perovskite film
FIG. 7 is an ultraviolet-visible-near infrared absorption spectrum of a perovskite light absorption layer on a magnetron sputtered zinc oxide/tin dioxide dual electron transport layer. As can be seen in fig. 7, the present invention can achieve a wide spectral response from visible to near-infrared.
Fig. 8 is a current-voltage (I-V) photovoltaic curve for a magnetron sputtered zinc oxide/tin dioxide dual electron transport layer based perovskite solar cell. As can be seen from fig. 8, the perovskite solar cell based on the magnetron sputtering zinc oxide/tin dioxide dual electron transport layer has better performance parameters, so as to obtain higher photoelectric conversion efficiency.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
1. putting a zinc oxide target material in a cavity, fixing FTO conductive glass above the target material, closing the cavity, vacuumizing, and adjusting oxygen to 6.0-8.0sccm and argon to 45-55sccm, wherein the pressure ratio is 1-3pa. Turning on a bipolar pulse power supply, and selecting the sputtering time to be 1-6 minutes; taking out the sputtering target from the cavity after sputtering;
2. and (3) spin-coating a perovskite layer and a hole layer on the magnetron sputtering zinc oxide single electron transmission layer, and finally evaporating a silver electrode, so as to obtain the perovskite solar cell based on the magnetron sputtering zinc oxide single electron transmission layer.
The perovskite light absorption layer is prepared by the following steps: 0.461g of lead iodide (PbI) was taken 2 ) And 0.159g of methyl amine iodide (CH) 3 NH 3 I) The drug was placed in a brown bottle, 635ul of Dimethylformamide (DMF) and 72ul of dimethyl sulfoxide (DMSO) were added dropwise to the bottle using pipette, respectively, and after adding a rotor, magnetic stirring was performed for 1 hour, followed by filtration to obtain a perovskite solution. And spin-coating the perovskite solution on a spin coater at the speed of 4000rmp/25s, dropwise adding an ethyl acetate anti-solvent at the 5 th s, and finally annealing at 70 ℃ for 20min to obtain the perovskite absorption layer. All the above operations were carried out in a glove box.
The preparation process of the cavity layer comprises the following steps: 72.3mg of Spiro-OMeTAD drug was dissolved in 1ml of chlorobenzene solution, followed by dropwise addition of 29ul of 4-tert-butylpyridine (4-TBP) and 18ul of Li-TFSI, followed by magnetic stirring with a rotor for 40min, and filtration to obtain a Spiro-OMeTAD solution. The resulting mixture was spin-coated with a Spiro-OMeTAD solution at a speed of 3000rmp/30s on a spin coater to obtain a hole layer. The above operation was also performed in a glove box.
3. And (3) testing the photoelectric conversion performance of the device of the perovskite solar cell obtained in the step (2), and the testing is shown in the following table 1.
Table 1 solar cell performance based on a single zinc oxide electron transport layer under different sputtering time conditions
| Sample numbering | Sputtering time (minutes) | Photoelectric conversion efficiency (%) |
| 1 | 1 | 10.1251 |
| 2 | 2 | 13.097 |
| 3 | 3 | 8.797 |
| 4 | 4 | 5.0567 |
| 5 | 5 | 4.41 |
| 6 | 6 | 3.441 |
As can be seen from table 1, different sputtering time parameters have a large impact on the performance of the corresponding solar cell.
Example 2:
1. putting a zinc oxide target material in a cavity, fixing FTO conductive glass above the target material, closing the cavity, vacuumizing, and adjusting oxygen to 6.0-8.0 and argon to 45-55 at a pressure ratio of 1-3pa. Turning on a bipolar pulse power supply, and selecting sputtering time for 2 minutes; taking out the sputtering target from the cavity after sputtering;
2. spin-coating the film prepared in the step 1 with a tin dioxide solution at 3000rmp/30s, and annealing for 30 minutes at 120-180 ℃ in the air to obtain a layer of tin dioxide film on the surface of the zinc oxide;
the tin dioxide solution is prepared by diluting tin dioxide hydrosol and water according to the volume ratio of 1-1.
3. And (3) coating a perovskite light absorption layer and a hole transport layer on the tin dioxide-zinc oxide double electron transport layer obtained in the step (2) in a spinning mode, and finally evaporating a silver electrode, so that the perovskite solar cell based on the tin dioxide and magnetron sputtering zinc oxide double electron transport layer is obtained.
The perovskite light absorption layer is prepared by the following steps: 0.461g of lead iodide (PbI) was taken 2 ) And 0.159g of methyl amine iodide (CH) 3 NH 3 I) The drug was placed in a brown vial, 635ul of Dimethylformamide (DMF) and 72ul of dimethyl sulfoxide (DMSO) were added dropwise to the vial using a pipette, respectively, and after adding the rotor, magnetic stirring was performed for 1 hour, followed by filtration to obtain a perovskite solution. And spin-coating the perovskite solution on a spin coater at the speed of 4000rmp/25s, dropwise adding an ethyl acetate anti-solvent at the 5 th s, and finally annealing at 70 ℃ for 20min to obtain the perovskite absorption layer. All the above operations were carried out in a glove box.
The preparation process of the cavity layer comprises the following steps: 72.3mg of Spiro-OMeTAD drug is dissolved in 1ml of chlorobenzene solution, 29ul of 4-tert-butylpyridine (4-TBP) and 18ul of Li-TFSI are sequentially added dropwise, then a rotor is added, magnetic stirring is carried out for 40min, and filtration is carried out, so as to obtain the Spiro-OMeTAD solution. The resulting mixture was spin-coated with a Spiro-OMeTAD solution at a speed of 3000rmp/30s on a spin coater to obtain a hole layer. The above operation was also performed in a glove box.
4. And (3) testing the photoelectric conversion performance of the device of the perovskite solar cell obtained in the step (3), and the testing is shown in the following table 2.
Table 2 solar cell performance based on tin dioxide and zinc oxide dual electron transport layers under different annealing conditions
| Sample numbering | Annealing temperature (. Degree.C.) | Photoelectric conversion efficiency (%) |
| 1 | 120 | 9.774 |
| 2 | 130 | 11.097 |
| 3 | 140 | 13.097 |
| 4 | 150 | 15.4589 |
| 5 | 160 | 14.1815 |
| 6 | 170 | 11.341 |
| 7 | 180 | 10.251 |
As can be seen from table 2, different annealing temperatures have a large impact on the performance of the corresponding solar cells.
Example 3:
1. putting a zinc oxide target material in a cavity, fixing FTO conductive glass above the target material, adjusting the distance between the target material and the FTO conductive glass to be 2-9 cm respectively, closing the cavity, vacuumizing, and adjusting 6.0-8.0sccm of oxygen, 45-55sccm of argon and the pressure ratio to be 1-3pa. Turning on a bipolar pulse power supply, and selecting sputtering time for 2 minutes; taking out the sputtering target from the cavity after sputtering;
2. spin-coating the film prepared in the step 1 with a tin dioxide solution at 3000rmp/30s, and annealing at 150 ℃ in air for 30 minutes to obtain a layer of tin dioxide film on the surface of zinc oxide;
the tin dioxide solution is prepared by diluting tin dioxide hydrosol and water according to the volume ratio of 1-1.
3. And (3) coating a perovskite layer and a hole layer on the double electron transport layer obtained in the step (2) based on the tin dioxide and the magnetron sputtering zinc oxide in a spinning mode, and finally evaporating a silver electrode, so that the perovskite solar cell based on the tin dioxide and the magnetron sputtering zinc oxide double electron transport layer is obtained.
The perovskite light absorption layer is prepared by the following steps: 0.461g of lead iodide (PbI) was taken 2 ) And 0.159g of methyl amine iodide (CH) 3 NH 3 I) The drug was placed in a brown bottle, 635ul of Dimethylformamide (DMF) and 72ul of dimethyl sulfoxide (DMSO) were added dropwise to the bottle using a pipette, respectively, and after adding a rotor, magnetic stirring was performed for 1 hour, followed by filtration to obtain a perovskite solution. And spin-coating the perovskite solution on a spin coater at the speed of 4000rmp/25s, dropwise adding an ethyl acetate anti-solvent at the 5 th s, and finally annealing at 70 ℃ for 20min to obtain the perovskite absorption layer. All the above operations were carried out in a glove box.
The preparation process of the cavity layer comprises the following steps: 72.3mg of Spiro-OMeTAD drug was dissolved in 1ml of chlorobenzene solution, followed by dropwise addition of 29ul of 4-tert-butylpyridine (4-TBP) and 18ul of Li-TFSI, followed by magnetic stirring with a rotor for 40min, and filtration to obtain a Spiro-OMeTAD solution. The resulting mixture was spin-coated with a Spiro-OMeTAD solution at a speed of 3000rmp/30s on a spin coater to obtain a hole layer. The above operation was also carried out in a glove box.
4. And (3) testing the photoelectric conversion performance of the device of the perovskite solar cell obtained in the step (3), and the testing is shown in the following table 3.
Table 3 solar cell performance based on different sputter spacing conditions of sample and target
| Sample numbering | Sputtering spacing (cm) | Photoelectric conversion efficiency (%) |
| 1 | 9 | 8.08 |
| 2 | 8 | 9.68 |
| 3 | 7 | 10.76 |
| 4 | 6 | 13.35 |
| 5 | 5 | 15.8251 |
| 6 | 4 | 14.312 |
| 7 | 3 | 12.15 |
| 8 | 2 | 9.01 |
As can be seen from table 3, the sputtering pitch has a large influence on the performance of the corresponding solar cell.
Claims (3)
1. A perovskite solar cell based on magnetron sputtering zinc oxide/tin dioxide double electron transport layers is characterized in that:
the perovskite solar cell adopts magnetron sputtering zinc oxide as an electron transmission layer, and tin dioxide is spin-coated to form the perovskite solar cell with double electron transmission layers, so that the mobility of the electron transmission layers is improved, the compactness of a film is improved, the carrier transmission is improved, and the photoelectric conversion efficiency and the stability of a device are improved;
the perovskite solar cell is prepared by a method comprising the following steps:
step 1: fixing a zinc oxide target material in a cavity, fixing FTO conductive glass above the target material, closing the cavity, sputtering zinc oxide by using a bipolar pulse power supply, adjusting oxygen to 6.0-8.0sccm, argon to 45-55sccm, and the air pressure to 1-3Pa, and taking out after sputtering is finished; the sputtering distance between the target and the FTO conductive glass is controlled to be 4-6cm; the sputtering time is 1-2 minutes;
and 2, step: spin-coating the film obtained in the step 1 with a tin dioxide solution for 3000rmp/30s, and then annealing in air to obtain a layer of tin dioxide film on zinc oxide; the tin dioxide solution is prepared by diluting a tin dioxide hydrosol and water according to a volume ratio of (1-1); the annealing is carried out at 150-160 ℃ for 30 minutes;
and step 3: and (3) spin-coating a perovskite light absorption layer and a hole transport layer on the tin dioxide-zinc oxide double electron transport layer obtained in the step (2), and finally evaporating a silver electrode, thereby obtaining the perovskite solar cell based on the tin dioxide and magnetron sputtering zinc oxide double electron transport layer.
2. The perovskite solar cell of claim 1, wherein:
in step 3, the perovskite light absorption layer is prepared by a method comprising the following steps: putting 0.461g of lead iodide and 0.159g of methyl amine iodide drug into a brown small bottle, respectively dropwise adding 635 mu L of dimethylformamide and 72 mu L of dimethyl sulfoxide into the bottle by using a liquid transfer gun, adding a rotor, magnetically stirring for 1 hour, and then filtering to obtain a perovskite solution; and spin-coating the perovskite solution on a spin coater at the speed of 4000rmp/25s, dripping an ethyl acetate anti-solvent at the 5 th s, and finally annealing at 70 ℃ for 20min to obtain the perovskite absorption layer.
3. The perovskite solar cell of claim 1, wherein:
in step 3, the hole transport layer is prepared by a method comprising the steps of: dissolving 72.3mg of Spiro-OMeTAD medicine into 1mL of chlorobenzene solution, sequentially dropwise adding 29 mu L of 4-tert-butylpyridine and 18 mu L of Li-TFSI, then adding a rotor, magnetically stirring for 40min, and filtering to obtain a Spiro-OMeTAD solution; the hole transport layer was obtained by spin-coating a Spiro-OMeTAD solution at a speed of 3000rmp/30s on a spin coater.
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| CN106935704A (en) * | 2016-12-02 | 2017-07-07 | 中国科学院合肥物质科学研究院 | A kind of method of electron transfer layer in utilization Ultra-Violet Laser treatment perovskite solar cell |
| WO2020029205A1 (en) * | 2018-08-09 | 2020-02-13 | 苏州大学张家港工业技术研究院 | Method for preparing inorganic perovskite battery based on synergistic effect of gradient annealing and antisolvent, and prepared inorganic perovskite battery |
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