CN109390471B - Method for preparing perovskite solar cell based on two-dimensional flower-shaped material molybdenum disulfide - Google Patents
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Abstract
The invention provides a method for preparing a perovskite solar cell based on a two-dimensional flower-shaped material molybdenum disulfide, which comprises the following steps: (1) depositing an electron transport layer TiO on the treated FTO substrate2(ii) a (2) Preparing a perovskite precursor solution; (3) depositing TiO on the perovskite precursor solution prepared in the step (2)2Preparing a film on the FTO substrate by using a spin coating method, and transferring the substrate to a heating table for annealing after spin coating; (4) adding a molybdenum disulfide precursor additive into a hole transport layer precursor solution, and preparing a hole transport layer by using a spin-coating method; (5) and (4) depositing a thin film of molybdenum trioxide and silver electrode on the hole transport layer prepared in the step (4) by utilizing a thermal evaporation technology. The method improves the photoelectric conversion efficiency and stability of the perovskite solar cell.
Description
Technical Field
The invention belongs to the field of photovoltaic devices, and particularly relates to a method for preparing a perovskite solar cell based on a two-dimensional flower-shaped material molybdenum disulfide.
Background
Planar organic-inorganic hybrid perovskite solar cells are widely spotlighted by their unique optical characteristics and simple fabrication processes. In recent years, a series of intensive researches on materials, thin film preparation technology, device structures and physical mechanisms have been carried out, and the photoelectric conversion efficiency of the photoelectric conversion device exceeds 22%. However, the research on the stability of the perovskite solar cell is relatively delayed, the defects of perovskite and device group materials cause that the perovskite solar cell cannot be produced in a large area and the performance stability of the device is poor, and the stability problem becomes a bottleneck for restricting the development of the perovskite solar cell. There are many factors that affect the lifetime stability of the device, including chemical stability due to the perovskite material itself and environmental conditions, and degradation of device performance due to ion migration at interfaces and between grain boundaries in the device components. The current common method for improving the stability of the perovskite battery is to insert an interface modification layer and dope a functional layer and a transmission layer to achieve the effect of interface passivation, but research on the stability of a device by a hole transmission layer is still very little, and further exploration is needed.
Disclosure of Invention
Aiming at the defects that the existing commonly-used additive for preparing a hole transport layer has ion migration phenomenon in the oxidation process, so that the stability defect of a thin film is more, the thin film is not compact, the perovskite at the lower layer is exposed and the like, the invention provides the method for preparing the perovskite solar cell based on the two-dimensional flower-shaped material molybdenum disulfide.
The invention adopts the following technical scheme that a method for preparing a perovskite solar cell based on a two-dimensional flower-shaped material molybdenum disulfide comprises the following preparation steps:
a method for preparing a perovskite solar cell based on a two-dimensional flower-shaped material molybdenum disulfide comprises the following steps:
(1) repeatedly ultrasonically cleaning an FTO transparent conductive glass substrate for three times by using deionized water, acetone and ethanol, and then baking for 20min until the solvent and the water are completely removed; then treating the treated FTO substrate with an ultraviolet lamp and ozone for 25min, and depositing an electron transport layer TiO on the treated FTO substrate2；
(2) 1mol of iodomethylamine (MAI) and lead iodide (PbI) were weighed out separately2) Adding 1mL of a mixed solvent consisting of dimethyl sulfoxide (DMSO) and gamma-butyrolactone (GBL), wherein the volume ratio of DMSO to GBL in the mixed solvent is 3: 7, preparing a perovskite precursor solution;
(3) depositing TiO in the step (1)2The FTO substrate is placed inTreating in an oxygen machine for 25min, taking out and transferring to a glove box, preparing a film on the substrate by the perovskite precursor solution prepared in the step (2) by using a spin coating method, and transferring the substrate to a heating table for annealing treatment after the spin coating;
(4) processing a hole transport layer 2,2',7,7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene (Spiro-OMeTAD) on the film prepared in the step (3) by a spin coating method; preparing molybdenum disulfide into a precursor additive by using an acetonitrile solvent, adding the molybdenum disulfide precursor additive into a hole transport layer precursor solution, and preparing a hole transport layer by using a spin coating method;
(5) depositing a thin film of molybdenum trioxide (MoO) on the hole transport layer prepared in the step (4) by utilizing a thermal evaporation technology3) And a silver electrode.
Further, TiO in the step (1)2The deposition method comprises the following steps: slowly dripping titanium tetrachloride into ice blocks frozen by ultrapure water, putting the ice blocks into a 70 ℃ oven when residual trace ice blocks are melted, carrying out deposition reaction for 1h, washing the substrate by the ultrapure water, putting the deposited substrate into a drying oven for later use, wherein the thickness of the film is 40 nm.
Further, the spin coating process in the step (3) is divided into two steps of low speed and high speed, and 180 mu L of chlorobenzene is dripped as an anti-solvent in the 20 th s of the high speed stage; standing for 5min, transferring the substrate to a heating table for annealing treatment, and annealing at 100 ℃ for 10 min.
Further, the spin coating conditions in the step (3) are 2000 rpm/20 s at a low speed, and then 4000 rpm/40 s at a high speed.
Further, the annealing process in the step (3) is 100 °/10 min.
Further, the adding mass fraction of the molybdenum disulfide precursor additive in the step (4) is 0.20-0.80 wt%.
Further, the spin coating condition in the step (4) is 5000 revolutions/40 s.
Further, no annealing treatment is required in the step (4).
Further, the thicknesses of the thin film molybdenum trioxide and the silver electrode in the step (5) are respectively 10nm and 100 nm.
Has the advantages that: the invention provides a method for preparing a perovskite solar cell based on a two-dimensional flower-shaped material molybdenum disulfide, which is used for improving the photoelectric conversion efficiency and stability of the perovskite solar cell, and the synthesized two-dimensional flower-shaped molybdenum disulfide is used as an additive to be inserted into a cavity transport layer precursor solution, and the method has the following advantages: (1) the synthesis method of the molybdenum disulfide is simple and the price of the required raw materials is low; (2) the material intervention method is simple and convenient, and the device preparation process is simple; (3) the recombination of electron holes in the hole transport layer is reduced, and the hysteresis phenomenon of the device is effectively improved; (4) effectively inhibit the migration of ions in the hole transport layer and prolong the service life of the device. The preparation process is simple and convenient, and the preparation difficulty is low; through the doping of flower-shaped molybdenum disulfide, the hole transport and stability of the hole transport layer are effectively improved, and through a series of gradient doping, the performance and stability of the device are obviously changed. The method is novel, the device manufacturing process is simple and convenient, the manufacturing difficulty is low, and the device performance is stable; through the intervention of the two-dimensional additive, the stability of the hole transport layer and the film coverage rate are effectively improved, and the performance of the device is remarkably changed through a series of gradient doping.
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The invention is further described with reference to the following figures and examples:
FIG. 1 is a schematic structural diagram of FIG. 1, wherein (a) is a schematic molecular structural diagram of additives for a hole transport layer, namely Li-TFSI (lithium bis (trifluoromethanesulfonylimide)) and molybdenum disulfide; FIG. 1 (b-c) is a scanning and transmission electron micrograph of molybdenum disulfide; FIG. 1 (d) is an X-ray diffraction pattern of molybdenum disulfide; fig. 1 (e) is a diagram of a hole transport layer precursor solution (molybdenum disulfide solution/molybdenum disulfide-free/molybdenum disulfide-containing hole transport layer precursor solution in this order from left to right).
FIG. 2 is a series of graphs representing the optical signals of thin films, and FIG. 2 (a) shows the UV-visible absorption of perovskite thin films and spin-coated Spiro-OMTAD doped and undoped molybdenum disulfide thin films; FIG. 2 (b) is a photoluminescence spectrum of a Spiro-OMTAD film doped with molybdenum disulfide and undoped; fig. 2 (c) is an electron spin resonance spectrum of a Spiro-OMTAD precursor solution doped with molybdenum disulfide and undoped; FIG. 2 (d) is a Hall effect spectrum of a Spiro-OMTAD film doped with molybdenum disulfide and undoped; FIG. 2 (e) shows J-V test patterns for a single hole device based on undoped and doped molybdenum disulfide Spiro-OMTAD films; FIG. 2 (f) shows a J-V diagram of a device based on undoped and doped molybdenum disulfide Spiro-OMTAD films in the dark state.
FIG. 3 is a scanning electron microscope image and an atomic force microscope image of a Spiro-OMTAD film doped with molybdenum disulfide and undoped, wherein (a) and (b) in FIG. 3 are respectively the film morphology images after a normal oxidation process under undoped and doped conditions; FIG. 3 (c) and (d) are the morphology of the film after storage for 72 hours under undoped and doped conditions, respectively; in FIG. 3, (e), (f) are atomic force micrographs after 72 hours of storage in undoped and doped conditions, respectively.
Figure 4 is a schematic representation of the principle of inhibiting ion migration by introducing molybdenum disulfide.
Fig. 5 is a longitudinal secondary ion mass spectrum of the film based on the undoped (a) in fig. 5 and the doped molybdenum disulfide (b) in fig. 5.
Fig. 6 is a graph of photoelectric characteristics of a perovskite solar cell device, wherein (a) in fig. 6 is a J-V curve of the device based on different doping ratios of molybdenum disulfide, (b) in fig. 6 is a statistical efficiency graph of a reference device, (c) in fig. 6 is an efficiency and current steady-state output curve of the device under an optimal doping ratio, (d) in fig. 6 is an external quantum efficiency graph of the reference device, (e) in fig. 6 is an efficiency lifetime graph of the reference device after being stored for 300 hours, and (f) in fig. 6 is a J-V curve of the reference device under forward and reverse scan voltages.
FIG. 7 is a J-V plot of the reference device after 72 hours storage at forward and reverse scan voltages (a); FIG. 7 (b) shows the J-V test pattern after 72 hours storage for a single hole device based on undoped and molybdenum disulfide doped Spiro-OMTAD films; FIG. 7 (c) is an electron spin resonance spectrum of a Spiro-OMTAD precursor solution undoped and doped with molybdenum disulfide under dark conditions and after storage for 72 hours; fig. 7 (d) shows the electron spin resonance spectra of undoped and doped molybdenum disulfide Spiro-omad precursor solutions under simulated sunlight irradiation for 5 minutes and after 72 hours of storage.
Detailed Description
The FTO transparent conductive glass substrates used in the following examples were purchased from Lumitec LTD2MAI was purchased from Sigma Aldrich and had a purity of greater than 99.999%.
Example 1: preparing a perovskite solar cell by using a molybdenum disulfide-doped hole transport layer precursor solution:
the synthesis method of the molybdenum disulfide comprises the following steps: 1.2410g (NH)4）6Mo7O24▪4H2O and 1.0629g of Thioacetamide CH3CSNH2The mixture was stirred for 0.5 hour until the solution was well mixed. The mixed solution was transferred to a 50mL Teflon reaction kettle and sintered at 220 ℃ for 6 hours. And repeatedly cleaning the obtained product with ethanol and ultrapure water for three times, and drying the obtained product in a vacuum drying oven at the temperature of 80 ℃ to obtain the final product.
The device structure of the battery is as follows: FTO/TiO2Perovskite layer (Perovskite)/Spiro-OMeTAD/MoO3/Ag
The preparation method of the hole transport layer precursor solution in this example is as follows: 5 mg of MoS2Dissolved in 3 mL of acetonitrile solvent and the solution after filtration appears pale blue. Then 15 mu L of the solution is taken to be added into Sprio-OMeTAD precursor solution, and the prepared solution is light blue (standard solution is light yellow). The preparation method of the perovskite precursor comprises the following steps: MAI and PbI2The molar ratio is 1: 1, namely, weighing 1mol of the mixture and adding the mixture into 1mL of mixed solvents DMSO and GBL respectively, wherein the volume ratio of the DMSO to the GBL in the mixed solvents is 3: 7.
the preparation process of the perovskite solar cell comprises the following steps:
(1) repeatedly ultrasonically cleaning the FTO transparent conductive glass substrate with deionized water, acetone and ethanol for three times, and then baking for 20min toCompletely removing the solvent and water; treating the treated FTO with ultraviolet lamp and ozone for 25min, and depositing the treated FTO with solution to form an electron transport layer TiO2，TiO2The deposition method comprises the following steps: slowly dripping 4.5 mL of titanium tetrachloride into ice blocks frozen by 200 mL of ultrapure water, putting the ice blocks into a 70 ℃ drying oven when residual trace ice blocks are melted, carrying out deposition reaction for 1h, washing the substrate by the ultrapure water, putting the deposited substrate into a drying oven for later use, wherein the thickness of the film is about 40 nm;
(2) deposit TiO well2The FTO substrate is placed in an ozone machine for ozone treatment for 25min, then taken out and transferred to a glove box, perovskite precursor solution is spin-coated on the substrate to form a film, the spin-coating method is used for preparing the film, the spin-coating process is divided into two steps, namely low speed 2000 r/20 s and high speed 4000 r/40 s, and 180 mu L of chlorobenzene is dropwise added at the 20 th s of the high speed stage to serve as an anti-solvent, so that the volatilization of the perovskite solvent is accelerated. Standing for 5min, and transferring the substrate to a heating table for annealing treatment, wherein the annealing process is 100 DEG/10 min.
(3) After the film is prepared, a hole transport layer Spiro-OMeTAD is prepared, wherein the preparation method is a spin coating method, the rotating speed is 5000 revolutions, and the spin coating time is 40 seconds. Adding different amounts of molybdenum disulfide precursor additives into the hole transport layer precursor solution respectively, preparing the hole transport layer by using a spin coating method, rotating for 5000 r 40s, and not annealing; the adding mass fractions of the molybdenum disulfide precursor additive are respectively 0.20 wt%, 0.40 wt%, 0.60wt% and 0.80 wt%.
Then the thermal evaporation technology is utilized to deposit the film MoO3And silver electrodes having a thickness of 10nm and 100nm, respectively.
(4) The J-V curve of the prepared perovskite solar cell is shown in figure 6, and it can be seen from the figure that the efficiency of the doped perovskite device is obviously improved, and the performance parameters are obviously improved. When the mass fraction of the doping material is 0.60wt%, the device exhibits optimized performance.
Fig. 2 shows the photoelectric properties of different prepared hole transport layers, and fig. 2 (a) (b) show absorption and emission spectrograms of undoped and doped molybdenum disulfide hole transport layers, respectively, and the combination of the spectrograms shows that the introduction of molybdenum disulfide is helpful for hole injection, and the recombination of electrons and holes at interfaces and layers is reduced. FIGS. 2 (c-d) show electron spin resonance and Hall effect spectra for undoped and doped molybdenum disulfide hole transport layers, respectively. Under the dark state condition, the doped solution presents stronger electronic signals, and the electronic signals are all enhanced along with the increase of the illumination time. Under the same illumination condition, the electron signal intensity of the doped solution is higher than that of the standard solution, so that the doped MoS2 has obvious influence on the electron state in the solution. The Hall effect can detect the change of the carrier signal in the sample more intuitively. Fig. 2 (e-f) shows J-V and dark J-V plots for undoped and doped molybdenum disulfide based hole transport layer single hole devices, respectively, where a significant decrease in the defect state of the doped device is observed, and the performance stability of the doped device is improved after storage for a period of time.
FIGS. 3 (a-b) are SEM images of undoped and doped molybdenum disulfide hole transport layers after a normal oxidation process, (c-d) are surface topography images of the films after 72 hours of storage, and (e-f) are AFM images of undoped and doped molybdenum disulfide hole transport layer films after 72 hours of storage. It is obvious from the appearance change that the undoped hole transport layer film is fast attenuated, a large number of holes and particles are arranged on the surface, and the surface of the film doped with molybdenum disulfide does not obviously change after being stored for a period of time. The perovskite crystal particles do not appear on the surface. The results are consistent with the AFM chart, and the roughness is not obviously changed.
Fig. 4 is a schematic diagram illustrating the principle of improving the stability of the perovskite battery, in which molybdenum disulfide can effectively adsorb lithium ions in the hole transport layer, inhibit the migration of ions to the perovskite layer, and slow down the attenuation of the perovskite layer during the oxidation storage process.
Fig. 5 shows secondary ion mass spectra of undoped and doped molybdenum disulfide hole transport layers, and it can be seen from the secondary ion mass spectra that after the undoped sample is stored for a period of time, the internal ions have obviously migrated, and the migration to the perovskite layer and the electron transport layer causes severe degradation of the device performance. After doping, the lithium ions are obviously fixed on the hole transport layer, so that the migration of the lithium ions is effectively inhibited, and the stability of the hole transport layer is very important.
Fig. 6 shows a series of characterizations of perovskite device performance for undoped and doped molybdenum disulfide hole transport layers. It can be seen from the figure that under the condition of doping 0.6wt%, the average efficiency of the device can reach 20%, and the positive and negative scanning results of the doped device have no big difference, i.e. the doping of the additive can effectively improve the hysteresis phenomenon of the battery device.
Fig. 7 shows a series of characterizations of the undoped and doped molybdenum disulfide hole transport layers after 72 hours of storage of the devices, from which it can be seen that the molybdenum disulfide doped precursor solution still has a higher electron signal after 72 hours of storage compared to the reference solution. And the stability of the device is obviously improved, and the hysteresis effect is also improved.
Claims (9)
1. A method for preparing a perovskite solar cell based on a two-dimensional flower-shaped material molybdenum disulfide is characterized by comprising the following steps:
(1) cleaning and drying an FTO transparent conductive glass substrate, then treating the treated FTO substrate by using an ultraviolet lamp and ozone, and depositing an electron transport layer TiO on the treated FTO substrate2；
(2) Respectively weighing 1mol of iodomethylamine and lead iodide, adding the iodomethylamine and the lead iodide into 1mL of mixed solvent consisting of dimethyl sulfoxide and gamma-butyrolactone, wherein the volume ratio of the dimethyl sulfoxide to the gamma-butyrolactone in the mixed solvent is 3: 7, preparing a pure iodine system perovskite precursor solution;
(3) depositing TiO in the step (1)2The FTO substrate is placed in an ozone machine for treatment, then taken out and transferred to a glove box, the perovskite precursor solution prepared in the step (2) is used for preparing a film on the substrate by using a spin coating method, and the substrate is transferred to a heating table for annealing treatment after being subjected to spin coating;
(4) processing a hole transport layer 2,2',7,7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene on the film prepared in the step (3) by a spin coating method; preparing molybdenum disulfide into a precursor additive by using an acetonitrile solvent, adding the two-dimensional flower-shaped molybdenum disulfide precursor additive into a hole transport layer precursor solution, and preparing a hole transport layer by using a spin-coating method;
(5) and (4) depositing a thin film of molybdenum trioxide and silver electrode on the hole transport layer prepared in the step (4) by utilizing a thermal evaporation technology.
2. The method for preparing the perovskite solar cell based on the two-dimensional flower-like material molybdenum disulfide according to claim 1, wherein TiO in the step (1)2The deposition method comprises the following steps: slowly dripping titanium tetrachloride into ice blocks frozen by ultrapure water, putting the ice blocks into a 70 ℃ oven when melting residual trace ice blocks, carrying out deposition reaction for 1h, washing the substrate by the ultrapure water, putting the deposited substrate into a drying box for later use, wherein the thickness of the titanium dioxide film is 40 nm.
3. The method for preparing the perovskite solar cell based on the two-dimensional flower-like material molybdenum disulfide as claimed in claim 1, wherein the spin coating process in the step (3) is divided into two steps of low speed and high speed, and 180 μ L of chlorobenzene is dropwise added as an anti-solvent at the 20 th s of the high speed stage; standing for 5min, transferring the substrate to a heating table for annealing treatment, and annealing at 100 ℃ for 10 min.
4. The method for preparing the perovskite solar cell based on the two-dimensional flower-like material molybdenum disulfide as claimed in claim 3, wherein the spin coating condition in the step (3) is that spin coating is performed at a low speed of 2000 rpm for 20s, and then spin coating is performed at a high speed of 4000 rpm for 40 s.
5. The method for preparing the perovskite solar cell based on the two-dimensional flower-like material molybdenum disulfide according to claim 1, wherein the annealing process in the step (3) is 100 ℃/10 min.
6. The method for preparing the perovskite solar cell based on the two-dimensional flower-shaped material molybdenum disulfide according to claim 1, wherein the molybdenum disulfide precursor additive is added in the step (4) in a mass fraction of 0.20-0.80 wt%.
7. The method for preparing the perovskite solar cell based on the two-dimensional flower-like material molybdenum disulfide according to claim 1, wherein the spin coating condition in the step (4) is 5000 revolutions per minute for 40 s.
8. The method for preparing the perovskite solar cell based on the two-dimensional flower-like material molybdenum disulfide according to claim 1, wherein an annealing treatment is not needed in the step (4).
9. The method for preparing the perovskite solar cell based on the two-dimensional flower-like material molybdenum disulfide as claimed in claim 1, wherein the thicknesses of the thin film molybdenum trioxide and silver electrode in the step (5) are 10nm and 100nm respectively.
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