CN108365102B - Stable and efficient two-dimensional layered perovskite solar cell and preparation method thereof - Google Patents
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Abstract
The invention discloses a method for preparing a stable and efficient two-dimensional layered perovskite solar cell in air, which is characterized in that the growth of micron-sized perovskite grains is realized by continuously heating in the whole spin coating process in the air, and a uniform and flat high-quality perovskite thin film and a stable and efficient perovskite photovoltaic device are prepared. The method of the invention, which is characterized in that the heating is continuously carried out in the whole spin coating process, enables the solvent to be volatilized quickly to accelerate the growth and the conversion of crystal grains, is also beneficial to the growth of two-dimensional layered perovskite along the direction vertical to the substrate, and finally forms a flat, compact and uniform perovskite thin film. The method disclosed by the invention does not need protection of inert atmosphere, is favorable for realizing large-area preparation of perovskite, and reduces cost.
Description
Technical Field
The invention relates to the field of perovskite solar cells, in particular to a stable and efficient two-dimensional layered perovskite solar cell and a preparation method thereof.
Background
In recent years, perovskite solar cells have been rapidly developed in the field of photovoltaic technology, the photoelectric efficiency of the perovskite solar cells is rapidly increased from the first 3.8% to 22.7% in a short period of several years, and the increasing speed is unprecedented in the field of photovoltaic technology. The perovskite material has the advantages of strong light absorption, high carrier mobility, long carrier diffusion distance, adjustable band gap and the like, so that the perovskite material is expected to become the most ideal solar cell material, and even the energy conversion efficiency of 33 percent is realized. Meanwhile, the perovskite solar cell can be prepared by a simple low-temperature solution method, and a bendable flexible device can be prepared on the flexible substrate.
At present, the perovskite solar cell with high efficiency is mainly of a three-dimensional structure, and the structure has excellent photoelectric properties, but is very sensitive to water, oxygen and light in the environment and has poor stability. The two-dimensional layered perovskite prepared by adding organic molecules such as long-chain amine or aromatic amine into the three-dimensional perovskite can greatly improve the hydrophobicity of the perovskite and the stability of the perovskite in the environment, and the band gap of the perovskite can be directly influenced by changing the amount of the organic molecules, so that the adjustable range of the band gap of the perovskite is greatly enlarged, and the perovskite material with an ideal band gap can be searched. The development prospect of the two-dimensional layered perovskite solar cell is very wide, whether from theoretical research or from future large-scale application.
It is worth noting that the grain growth of the perovskite and the morphology of the thin film are critical to improve the efficiency of the perovskite thin film. According to the traditional preparation method of the two-dimensional layered perovskite thin film, the obtained perovskite crystal grains grow towards the direction which is not beneficial to carrier transmission, so that the efficiency of the device is extremely low. At present, the two-dimensional layered perovskite solar cell with the highest efficiency needs to adopt a substrate preheating mode to prepare the perovskite thin film, the substrate temperature of the mode is difficult to control in the spin coating process, the repeatability is poor, and the technical requirement on operators is higher. Meanwhile, the thickness of the prepared perovskite thin film is not uniform and the uniformity is poor due to the fact that the temperature of the substrate is not uniform. Moreover, the preparation process of the two-dimensional layered perovskite is basically carried out in an inert atmosphere at present, which is not beneficial to industrial mass production.
Disclosure of Invention
The invention aims to provide a method for preparing two-dimensional layered perovskite in air and realize a high-efficiency and stable perovskite solar cell.
The traditional method for preparing perovskite at room temperature is not beneficial to growth of perovskite grains towards a beneficial direction, and has the problems of slow solvent volatilization, more residues and the like. The substrate preheating method has the problems of non-uniform substrate temperature and non-uniform solvent volatilization speed. In order to overcome the problems, the invention adopts ionic liquid with lower boiling point as solvent, uses the mode of continuously heating and stabilizing the whole spin coating process in a proper temperature range, and realizes the rapid and uniform volatilization of the solvent by adjusting the solubility, the spin coating rotating speed, the spin coating temperature and time, and the annealing time and temperature of the two-dimensional layered perovskite, thereby effectively regulating and controlling the average grain size of the two-dimensional layered perovskite, simultaneously leading the grains to grow towards the direction vertical to the substrate, finally obtaining the film with uniform, compact and high crystallinity on the surface, and improving the photoelectric conversion efficiency and stability of the perovskite. In addition, for the traditional solvents such as N, N-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and the like, the toxicity of the used ionic solvents such as methylamine acetate (MAAc) and methylamine formate (MAFA) is greatly reduced, and the environment is more friendly; the whole two-dimensional layered perovskite film is completely carried out in the air, so that the production cost is reduced, and the method is more favorable for industrial large-scale production.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a preparation method of a stable and efficient two-dimensional layered perovskite solar cell is characterized in that the preparation process of a perovskite light absorption layer is completely carried out in the air, the whole process is continuously heated, the device structure of the perovskite solar cell sequentially comprises a transparent conductive substrate, a hole transmission layer, the perovskite light absorption layer, an electron transmission layer, an interface modification layer and a metal electrode, the hole transmission layer and the electron transmission layer are prepared by a solution method, the interface modification layer and the metal electrode are prepared by a thermal evaporation deposition method, and the preparation of the perovskite light absorption layer comprises the following steps:
a. dissolving metal halide, methylamine salt and macromolecular amine salt in a solvent according to a stoichiometric ratio (n: n-1:2, n is 1 to infinity, n belongs to R), and stirring for 1-18h at 60 ℃ to obtain a clear and transparent perovskite precursor solution; the concentration of the perovskite precursor solution is 100-400 mg/ml;
b. preheating a precursor solution at 60 ℃ in the air, dropwise adding 70-200 mu L of the precursor solution onto a 60-200 ℃ substrate, and quickly spin-coating for 10 s-3 min at the rotation speed of 2000-8000rmp, wherein the substrate temperature is kept at 60-200 ℃ in the whole spin-coating process to obtain a uniform and smooth perovskite thin film;
c. annealing the obtained perovskite thin film at 60-150 ℃ for 0-10 min to obtain the high-quality two-dimensional layered perovskite thin film.
Preferably, the transparent conductive substrate is one of ITO conductive glass or polyethylene terephthalate (PET).
Preferably, the hole transport layer is poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS), CuSCN, CuI, NiOxThe electron transport layer is one of fullerene derivatives PCBM or ZnO, and the interface modification layer is LiF or MoO3、BCP、C60In one of the metal electrodes, the metal electrode is one of Al, Ag or Au.
Preferably, the solvent used for the perovskite light absorption layer precursor solution is one or a mixture of DMF, DMSO and MAAc.
Preferably, the perovskite light-absorbing layer is A'2An-1MnX3n+1(n ═ 1 to infinity, n ∈ R), wherein A' is long-chain amine ions or aromatic amine ions, A is methylamine ions, M is metal ions such as lead and tin, and X is one or more of Cl, Br and I.
Has the advantages that: compared with other preparation methods of perovskite solar cells, the preparation method can prepare the perovskite active layer in the air, is completely free from the influence of environmental factors, adopts an organic solvent with low toxicity, and accords with the concept of green chemistry. In addition, the crystal grains of the two-dimensional perovskite thin film prepared by the method grow along the direction vertical to the substrate, the crystal grains are larger, the defects are fewer, the short-circuit current is obviously improved, and the stable and efficient two-dimensional perovskite solar cell can be realized. These characteristics are very advantageous for large-scale commercial applications.
Drawings
Fig. 1 is a schematic structural diagram of a high-efficiency stable two-dimensional layered perovskite solar cell in an embodiment of the invention.
Fig. 2 is a J-V curve and photoelectric property parameters of a two-dimensional layered perovskite solar cell manufactured by using a substrate preheating method with conventional DMF as a solvent in an embodiment of the present invention, and an atomic force microscope image of a two-dimensional layered perovskite thin film manufactured by using a substrate preheating method with conventional DMF as a solvent.
FIG. 3 is a J-V curve and photoelectric property parameters of a two-dimensional layered perovskite solar cell prepared by heating and spin-coating MAAc as a solvent in an embodiment of the invention, and an atomic force microscope image of a two-dimensional layered perovskite thin film prepared by heating and spin-coating MAAc as a solvent in the embodiment of the invention.
FIG. 4 is a scanning electron micrograph of the surface of a two-dimensional layered perovskite thin film prepared by substrate preheating
Detailed description of the invention
Example 1
The invention provides a high-efficiency stable two-dimensional layered perovskite solar cell, which sequentially comprises a conductive transparent substrate (ITO, PET and the like), a hole transport layer (PEDOT: PSS, CuI, CuSCN and NiO)XRGO, GO, etc.), two-dimensional layered perovskite active layer A'2An-1MnX3n+1(n 1 to infinity), electron transport layer (PCBM, ZnO, etc.), interface modification layer (LiF, MoO)3、BCP、C60Etc.), metal electrodes (Au, Ag, Al, etc.).
The invention provides a method for preparing a two-dimensional layered perovskite solar cell in air, which mainly comprises the following operation steps:
the method comprises the following steps: the conductive transparent substrate treated by the cleaning process is blow-dried with nitrogen gas and subjected to hydrophilic treatment.
Step two: and depositing a hole transport layer on the conductive transparent substrate obtained by the first step through a solution spin coating process.
Step three: and (4) placing the device obtained through the second step on a heating spin-coating instrument, and continuously depositing a two-dimensional layered perovskite active layer through a heating spin-coating process.
Step four: and transferring the device obtained through the third treatment step into an inert atmosphere, and continuously depositing an electron transport layer on the surface through a solution spin coating process.
Step five: and transferring the device obtained by the fourth treatment step into evaporation equipment, and depositing an interface modification layer and a metal electrode at a certain rate.
The first step comprises the following steps: a. the conductive transparent substrate is one of ITO or PET; b. ultrasonically cleaning with detergent, deionized water, acetone and ethanol for 20min, and blow-drying with nitrogen gun; c. and treating the transparent substrate with an ultraviolet ozone machine for 15-30 min.
The second step comprises the following steps: a. one or more of PETDOT, PSS, CuSCN, CuI, NiOx, RGO, GO and the like are selected to form a composite material which is prepared into solution with a certain concentration in advance. b. And (3) depositing a hole transport layer with the thickness of 10 nm-100 nm on the conductive transparent substrate treated in the step one by adopting a spin coater at a certain spin-coating rotating speed and time.
The third step comprises the following steps: a. mixing the macromolecular amine salt, MACl and PbI2Preparing 150mgmL according to the stoichiometric ratio-1～350mg mL-1Stirring the perovskite precursor solution for 1 to 24 hours at the temperature of between 50 and 80 ℃; b. spin-coating at 3000-6000 rmp for 10 s-1 min in air at 60-130 deg.C to obtain two-dimensional layered perovskite thin film on the surface during the step three treatment, and step annealing at 60-100 deg.C for 3-10 min.
The fourth step comprises the following steps: a. selecting one or more of PCBM, ZnO and other materials to prepare a composite material into a solution with a certain concentration in advance; b. and (3) depositing an electron transmission layer with the thickness of 10 nm-100 nm on the conductive transparent substrate treated in the step one by adopting a spin coater at a certain spin-coating rotating speed and time.
The fifth step comprises the following steps: a. pumping the vacuum degree to<5×10-4Pa; b. MoO3, LiF, BCP and C are selected60One of the materials is used as an interface modification layer material, one of Au, Ag, Al and the like is selected as a metal electrode material, and the like
The thickness of the interface modification layer material is about 1-10 nm and the thickness of the metal electrode is 80-150 nm.
Example 2
The structure of the two-dimensional layered perovskite solar cell in the embodiment of the invention is shown in fig. 1, and the two-dimensional layered perovskite solar cell is sequentially arranged as follows: ITO transparent conductive glass, hole transport layer (PEDOT: PSS), two-dimensional layered perovskite active layer (BA)2MA3Pb4IXCl13-x) The electron transport layer (PCBM), the interface modification Layer (LiF) and the metal electrode (Al).
1. Treatment of two-dimensional layered perovskite solar cell conductive transparent substrate
(1) Carrying out ultrasonic treatment on the ITO transparent conductive glass for 20min by using a detergent once, and respectively carrying out ultrasonic treatment on deionized water, acetone and ethanol for 10 min; (2) and (3) treating the cleaned ITO transparent conductive glass in an ultraviolet ozone machine for 20 min.
2. Preparation of hole transport layer of two-dimensional layered perovskite solar cell
(1) PSS as a hole transport layer material is firstly filtered by a 0.22-micron water system filter head, and then transferred to the ITO conductive glass surface treated in the step 1 by a liquid transfer gun to be paved on the surface. (2) And spin-coating for 30-60 s by using a spin-coating instrument at a rotating speed of 3000-5000 rmp, and annealing at 120-140 ℃ for 15-30 min after the spin-coating is finished to obtain the perovskite hole transport layer with the thickness of about 50 nm.
3. Preparation of two-dimensional layered perovskite solar cell photoactive layer
(1) The traditional DMF is taken as a solvent and is prepared by adopting a substrate preheating mode
a. Mixing BAI, MACl, PbI2Dissolving the mixture in DMF according to the molar ratio of 2:3:4, stirring the mixture for 1 to 24 hours at the temperature of 60 ℃ to prepare 200mg mL-1The precursor solution of (1); b. preheating the precursor solution to 50-100 ℃, preheating the device prepared in the step 1 to 60-130 ℃, quickly transferring the hot substrate to a room-temperature spin coater, fully spreading the precursor solution, spin-coating for 10-60 s, and performing gradient annealing at 60-100 ℃ for 3-10 min.
(2) MAAc is used as solvent and is prepared by adopting a heating spin coating mode
a. Mixing BAI, MACl, PbI2Dissolving in MAAc according to the molar ratio of 2:3:4, stirring at 60 ℃ for 1-24 h to obtain 200mg mL-1The precursor solution of (1); b. preheating the precursor solution to 50-100 ℃, transferring the device prepared in the step 1 to a heating spin-coating instrument at 60-130 ℃, fully spreading the precursor solution, spin-coating for 10-60 s, continuously heating in the whole spin-coating process, and carrying out gradient annealing at 60-100 ℃ for 3-10 min.
4. Preparation of two-dimensional layered perovskite solar cell electron transport layer
(1) Dissolving the electron transport layer material PCBM in anhydrous chlorobenzene, preparing a solution with the concentration of 10-30 mg/ml, and magnetically stirring for 24 hours at the temperature of 60-70 ℃; (2) transferring the device prepared in the step (3) to an inert atmosphere; (3) taking out the prepared PCBM solution by using a liquid transfer gun, dripping the PCBM solution on the surface of the device processed in the step 3, and spin-coating for 30-60 s by using a spin coater at the rotating speed of 1000-3000 rmp.
5. Preparation of two-dimensional layered perovskite solar cell interface modification layer and metal electrode
(1) Transferring the device prepared in the step 4 into evaporation equipment, and pumping the vacuum degree to<5×10-4Pa; (2) firstly, use
At a rate of 1nm to 10nm, and then
The rate of the Al electrode is 80 nm-150 nm.
6. Testing surface morphology of two-dimensional layered perovskite active layer and testing performance parameters of two-dimensional layered perovskite solar cell
The cross-sectional morphology of the two-dimensional layered perovskite active layer is tested by adopting a JSM-7800F scanning electron microscope, as shown in figures 2 and 3, the perovskite active layer prepared by using MAAc as a solvent and adopting a heating spin coating method has obviously large crystal grains, the crystallization quality of the film is improved, and the surface is more compact and smooth.
The performance parameters of the two-dimensional layered perovskite solar cell were tested by using a solar simulator (Oriel Newport, 150W, AM 1.5) as a light source, and the light intensity was calibrated with a standard silicon reference cell (Oriel Newport PN 91150V). The intensity is 100mW cm-2(AM 1.5) simulated sunlight was incident from the anode of the two-dimensional layered perovskite solar cell, and the photocurrent-voltage curve of the cell was recorded using a Keithley2400 digital source meter. As shown in FIG. 2 and FIG. 3, the test results of the photoelectric performance parameters of the cell are shown, and it can be seen that the two-dimensional layered perovskite active layer prepared by using MAAc as a solvent and adopting a heating spin coating method is electrically connectedThe photoelectric conversion efficiency of the cell is obviously improved.
The embodiments of the present invention have been described in detail in the above examples, but the present invention is not limited to the specific details in the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
Claims (4)
1. The preparation method of the stable and efficient two-dimensional layered perovskite solar cell is characterized in that the preparation process of the perovskite light absorption layer is completely carried out in the air, the whole process is continuously heated, the device structure of the perovskite solar cell sequentially comprises a transparent conductive substrate, a hole transmission layer, the perovskite light absorption layer, an electron transmission layer, an interface modification layer and a metal electrode, the hole transmission layer and the electron transmission layer are prepared by a solution method, the interface modification layer and the metal electrode are prepared by a thermal evaporation deposition method, and the preparation of the perovskite light absorption layer comprises the following steps:
a. dissolving metal halide, methylamine salt and macromolecular amine salt in a solvent according to a stoichiometric ratio (n: n-1:2, n is 1 to infinity, n belongs to R), and stirring for 1-18h at 60 ℃ to obtain a clear and transparent perovskite precursor solution; the concentration of the perovskite precursor solution is 100-400 mg/ml;
b. preheating a precursor solution at 60 ℃ in the air, dropwise adding 70-200 mu L of the precursor solution onto a 60-200 ℃ substrate, and quickly spin-coating for 10 s-3 min at the rotation speed of 2000-8000rmp, wherein the substrate temperature is kept at 60-200 ℃ in the whole spin-coating process to obtain a uniform and smooth perovskite thin film;
c. annealing the obtained perovskite thin film at 60-150 ℃ for 0-10 min to obtain a high-quality two-dimensional layered perovskite thin film;
the solvent used by the perovskite light absorption layer precursor solution is MAAc.
2. The method according to claim 1, wherein the transparent conductive substrate is one of ITO conductive glass or polyethylene terephthalate (PET).
3. The method for preparing the stable high-efficiency two-dimensional layered perovskite solar cell as claimed in claim 1, wherein the hole transport layer is poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS), CuSCN, CuI, NiOxThe electron transport layer is one of fullerene derivatives PCBM or ZnO, and the interface modification layer is LiF or MoO3、BCP、C60In one of the metal electrodes, the metal electrode is one of Al, Ag or Au.
4. The method of claim 1, wherein the perovskite light-absorbing layer is A'2An-1MnX3n+1(n ═ 1 to infinity, n ∈ R), wherein A' is long-chain amine ions or aromatic amine ions, A is methylamine ions, M is metal ions such as lead and tin, and X is one or more of Cl, Br and I.
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