CN115275026A - 2D/3D perovskite solar cell and preparation method thereof - Google Patents
2D/3D perovskite solar cell and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of solar cells, and discloses a 2D/3D perovskite solar cell and a preparation method thereof, wherein a glass slide is additionally arranged on the surface of a 2D perovskite layer to ensure that a PEAI solution is fully contacted with the surface of the 3D perovskite, a PEAI is used as a 2D perovskite barrier layer, a 2D covering layer is grown in situ on the top of a 3D perovskite film, the annealing method of the 2D layer and the PEAI concentration are improved, and low-temperature carbon slurry is used for replacing a hole transport layer HTM and a metal electrode, so that the 2D/3D perovskite solar cell is prepared. The invention uses the low-temperature carbon slurry to replace an expensive hole transport layer HTM and a metal electrode, avoids the mutual permeation of the metal electrode and a perovskite layer after being placed for a long time, and greatly reduces the experiment cost. The perovskite battery prepared by the method has low cost and remarkably improved thermal stability, can still keep 90% of the initial efficiency after being heated for 10 hours at 70 ℃, and has the photoelectric efficiency of 14.63%.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a 2D/3D perovskite solar cell and a preparation method thereof.
Background
Perovskite is one of the most studied and promising photovoltaic materials due to its advantages of excellent photovoltaic performance, tunable energy band, high light absorption coefficient, and low exciton binding energy. Perovskite solar cells (PeSCs) have achieved surprising achievements in photoelectric conversion in the last decade, with the highest certified Photoelectric Conversion Efficiency (PCE) of perovskite solar cells reaching 25.7%, approaching the shokrill-quinse limit. Perovskite cells have shown good application prospects in the next generation of photovoltaic devices. However, some challenges need to be addressed before commercial production, such as large defects in surface formation, resulting in severe non-radiative recombination, and insufficient material interactions between the components, resulting in thermal, humidity, and light-induced degradation.
Two-dimensional perovskites are a new class of photovoltaic materials in which organic layers serve as protective barriers against moisture or ion attack, and have recently emerged and attracted increasing attention because they exhibit significant stability. Inspired by this, the use of two-dimensional perovskite deposited on top of three-dimensional perovskite for surface passivation triggered a new wave of research to achieve both higher efficiency and stability. The structure remarkably improves the stability of the PSC and the photoelectric property of the cell without affecting the high performance of the PSC by growing the 2D covering layer on the top of the 3D perovskite thin film in situ. Currently, PSCs have achieved significant performance with the help of two-dimensional perovskite surface passivation. For example, poplar et al employed the newly designed cyclohexylethylammonium iodide (CEAI) as a 3D perovskite surface passivating agent. By reducing trap-assisted recombination through the formation of a 2D perovskite layer, the fill factor is increased to 82.6%, and thus the PCE is increased by 23.57%. The introduced CEAI also improved the surface hydrophobicity, keeping the residual efficiency of the passivated device above 96% at 1 sun after 1500 hours. Record-creating certification efficiency (25.2%) of PSCs obtained by gold and coworkers was also based on 2D perovskite passivation films. The basic light absorbing layer is a 2D/3D heterojunction induced by Octyl Ammonium Iodide (OAI) and n-hexyl ammonium. In addition, king et al successfully created thermodynamically stable all-inorganic (β -CsPbI 3-based) PSCs with >18% efficiency by using choline iodide (CHI) in crack-filling interface engineering. In the aspect of carbon electrode-based perovskite batteries, the german Wagner group introduced a two-dimensional perovskite passivation layer (OAI) as an electron blocking layer, significantly reducing interfacial recombination losses. This allows an efficiency of 18.5% for HTM-free printable low temperature carbon electrode perovskite solar cells using two-dimensional perovskites as electron blocking layers and significantly improves device stability.
Compared with the traditional 3D perovskite cell, the 2D/3D perovskite cell has more excellent performance and greatly improved stability, and is beneficial to commercialization of perovskite solar cells.
Through the above analysis, the problems and defects of the prior art are as follows: during the perovskite film forming process, a large amount of grain boundary and interface defects are generated due to the existence of dangling bonds on grain boundaries and crystal planes. These detrimental defects severely affect carrier transport, resulting in severe non-radiative recombination. Meanwhile, perovskite materials have different degrees of decomposition phenomena due to insufficient interaction among the components, and the decomposition process of the perovskite materials is accelerated particularly when the perovskite materials are exposed to high humidity, high temperature, strong light, oxygen enrichment and the like. There has been a significant improvement in the stability of PSCs under conventional conditions and the photovoltaic performance of the cells without compromising their high performance by growing a 2D overlayer in situ on top of a 3D perovskite thin film. However, the stability of perovskite cells under high temperature, high humidity, light, etc. is still lacking.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a 2D/3D perovskite solar cell and a preparation method thereof, and particularly relates to an improved 2D layer annealing method.
The invention is realized in such a way that a preparation method of a 2D/3D perovskite solar cell comprises the following steps:
and adding a glass slide on the surface of the 2D perovskite layer to ensure that a PEAI solution is fully contacted with the surface of the 3D perovskite, using PEAI as a 2D perovskite barrier layer, growing a 2D covering layer on the top of the 3D perovskite film in situ, improving the annealing method of the 2D layer and the PEAI concentration, and using low-temperature carbon slurry to replace a hole transport layer HTM and a metal electrode, thereby preparing the 2D/3D perovskite solar cell.
Further, the preparation method of the 2D/3D perovskite solar cell comprises the following steps:
step one, manufacturing an electron transport layer comprising TiO 2 Dense layer, tiO 2 Nanoarrays and SnO 2 Layer manufacturing;
step two, respectively manufacturing a perovskite layer and a 2D layer;
and step three, manufacturing the C electrode by adopting a screen printing process.
Further, tiO in the first step 2 The preparation of the compact layer comprises the following steps:
respectively carrying out ultrasonic treatment on the conductive glass FTO for 30min by using washing powder, deionized water, acetone and ethanol, and blow-drying the FTO from the side by using a clean nitrogen gun after cleaning is finished; after a yellow adhesive tape is pasted on the conductive surface of the glass to reserve a reserved electrode, placing the substrate under an ozone cleaning machine, and cleaning for 30min; 2.2mL of titanium tetrachloride is dropwise added into 200mL of ice-water mixture, the mixture is stirred and melted, the solution is clear and transparent, and the prepared TiCl 4 The concentration of the solution is 0.1M to obtain cp-TiO 2 The precursor solution of (1); placing the FTO treated by ozone into a clean glass culture dish, and slowly pouring the prepared TiCl 4 Precursor solution, putting the sealed culture dish into a water bath kettle heated to 70 ℃, taking out after reacting for 2h, and standing for 30min; after cooling to room temperature, cleaning with deionized water, annealing at 150 deg.C for 2h 2 And finishing the sample preparation.
Further, tiO in the first step 2 The preparation of the nano array comprises the following steps:
preparing a mixture with a volume ratio of 1:1, 100mL of hydrochloric acid deionized water mixed solution, sealing tightly and placing on a magnetic stirrer at normal temperatureStirring for 30min, slowly dripping 1.5mL of tetrabutyl titanate solution after stirring is finished, and fully stirring to obtain a precursor solution; the prepared cp-TiO 2 Transferring the sample into a liner of a reaction kettle, placing the conductive glass surface upwards, pouring the stirred precursor solution into the reaction kettle, and heating the mixture in a drying oven at 150 ℃ for 105min; after the reaction time is over, taking out the sample, cleaning the sample by using deionized water, placing the sample in a muffle furnace for annealing at 150 ℃ for 2h 2 And completing the NA preparation.
Further, snO in the first step 2 The layer fabrication includes:
1mL of tin tetrachloride was added to 200mL of deionized water and stirred until complete fusion. The preparation method is the same as that of TiO 2 A dense layer.
Further, the perovskite layer manufacturing in the second step includes:
weighing a certain amount of PbI 2 Dissolving the powder in a mixed solvent of DMF and DMSO, and V: v =9:1, preparing PbI 2 The solution with concentration of 1.5M is placed on a magnetic stirrer and heated and stirred for 30min at 70 ℃; respectively taking 6.39mg, 9mg and 90mg of iodomethylamine, chloromethane and iodoformamidine powder, adding 1mL of isopropanol solution into the mixed medicine powder, and continuously shaking on a shaking instrument for 15min; the first step of the two-step spin coating method is to spin-coat PbI 2 Solution, using pipette gun to take 50 μ L of PbI 2 The solution is dropped on the surface of the substrate after UV; the spin coating time is 30s at the spin coating speed of 1500rpm, and the annealing is carried out for 10s on a hot bench at the temperature of 70 ℃; spin-coating an organic salt solution, taking 50 mu L of organic salt to spin-coat on a sample, wherein the spin-coating rotation speed is 1500rpm, and the spin-coating time is 30s; and immediately taking down the film after the spin coating, placing the film on a constant-temperature heating table at 150 ℃ for annealing for 30min, and finishing the preparation of the PeSK film.
Further, the 2D layer in step two is made by:
spin-coating PEAI solution on the prepared perovskite layer for post-treatment, wherein the concentration of the PEAI solution is 10mg/mL; the PEAI spin coating speed is 5000rpm, the acceleration is 9000rpm, and the time is 30s; covering the glass slide on the upper surface after the spin coating is finished so that the perovskite is fully contacted with the PEAI solution, and annealing for 10min in a constant temperature heating table at 100 ℃; and cooling to room temperature and taking down the glass cover plate.
Further, the C electrode in step three is fabricated by:
and transferring the low-temperature carbon slurry onto the 2D-3D layer by adopting a screen printing process, and immediately annealing for 10min on a constant-temperature heating table at 100 ℃ after the transfer process is finished.
Furthermore, the preparation process of the 2D/3D perovskite solar cell is carried out in the air, the temperature is 25-28 ℃, and the humidity is 27-30%.
The invention also aims to provide a 2D/3D perovskite solar cell prepared by implementing the preparation method of the 2D/3D perovskite solar cell.
In combination with the above technical solutions and the technical problems to be solved, please analyze the advantages and positive effects of the technical solutions to be protected in the present invention from the following aspects:
first, aiming at the technical problems existing in the prior art and the difficulty in solving the problems, the technical problems to be solved by the technical scheme of the present invention are closely combined with results, data and the like in the research and development process, and some creative technical effects are brought after the problems are solved. The specific description is as follows:
aiming at the problems of the perovskite battery and the defects of the prior art, the 2D covering layer grows on the top of the 3D perovskite thin film in situ, so that the stability of the PSC and the photoelectric performance of the battery are obviously improved under the condition of not influencing the high performance of the PSC. At present, the manufacturing process of 2D/3D perovskite is mature gradually, and most researches only concern about the stability of the device under the normal-temperature dry environment. The devices are required to face conditions such as high temperature and high humidity, which are essential for industrialization, but the 2D/3D perovskite has poor stability under the conditions of light, high temperature and high humidity. According to the invention, PEAI is used as a 2D perovskite barrier layer, and by improving the annealing method of the 2D layer, a glass slide is added on the surface of the 2D perovskite layer during annealing so that PEAI solution is fully contacted with the surface of the 3D perovskite layer, and meanwhile, the glass cover plate reduces the volatilization of the PEAI solution so that a flat 2D perovskite layer is formed on the surface of the PEAI solution. Surface morphology tests show that the 2D/3D perovskite film has smooth surface morphology, no obvious defects and compact and uniform grain arrangement. The light absorption capacity is obviously improved. Meanwhile, the XRD shows that the 2D/3D perovskite thin film has no yellow phase, and the ratio of the perovskite peak value to the residual lead iodide peak value is obviously reduced compared with that of the 3D perovskite, so that the quality of the 2D/3D perovskite thin film is obviously improved. The 2D/3D perovskite battery covered with the glass cover plate has higher stability in the severe environments of illumination, high temperature, high humidity and the like than the 3D perovskite battery, and the efficiency is still 90 percent of the initial efficiency after the battery is heated for 10 hours at 70 ℃. The experiment is completely made in the air, and the experimental process is more convenient. Meanwhile, the low-temperature carbon slurry is used for replacing an expensive hole transport layer HTM and a metal electrode, so that the metal electrode and a perovskite layer are prevented from mutually permeating after being placed for a long time, and the experiment cost is greatly reduced.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows:
the perovskite battery prepared by the method has low cost and remarkably improved thermal stability, can still keep 90% of the initial efficiency after being heated for 10 hours at 70 ℃, and has the photoelectric efficiency of 14.63%.
Thirdly, as the creative auxiliary evidence of the claims of the present invention, it is also reflected in that the technical solution of the present invention solves the technical problem which people have eagerly solved but have not succeeded all the time:
the manufacturing process of 2D/3D perovskite is gradually mature, and the essential requirements for the industrialization of perovskite solar cells face the conditions of light, high temperature, high humidity and the like, and the stability under these conditions is a great challenge for the industrialization of perovskite cells. However, at present, no relatively perfect solution to this problem exists. The invention provides an annealing method for improving a 2D/3D perovskite battery, which improves the stability of the battery under the conditions of illumination, high temperature, high humidity and the like, and has simple operation and low cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a method for fabricating a 2D/3D perovskite solar cell according to an embodiment of the invention;
FIG. 2 is an SEM surface view of a perovskite thin film provided by an embodiment of the invention;
FIG. 3 is a block diagram of a perovskite battery provided by an embodiment of the invention;
FIG. 4 is a graph of the UV-vis absorption spectrum of a 2D/3D perovskite layer provided in an embodiment of the present invention;
FIG. 5 is an XRD pattern of a perovskite layer provided by an embodiment of the present invention;
FIG. 6 is a J-V plot of a 2D/3D perovskite battery provided by an embodiment of the invention;
FIG. 7 is a graph of the thermal stability of a 2D/3D perovskite battery provided by an embodiment of the invention;
FIG. 8 is a graph of the stability of a 2D/3D perovskite cell provided by an embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In view of the problems in the prior art, the present invention provides a 2D/3D perovskite solar cell and a method for manufacturing the same, which will be described in detail below with reference to the accompanying drawings.
1. Illustrative embodiments are explained. This section is an illustrative example developed to explain the claims in order to enable those skilled in the art to fully understand how to implement the present invention.
As shown in fig. 1, a method for manufacturing a 2D/3D perovskite solar cell according to an embodiment of the present invention includes the following steps:
s101, electronic transmissionMaking of transfer layers, including TiO 2 Dense layer, tiO 2 Nanoarrays and SnO 2 Layer manufacturing;
s102, respectively manufacturing a perovskite layer and a 2D layer;
and S103, manufacturing the C electrode by adopting a screen printing process.
As a preferred embodiment, the method for manufacturing a 2D/3D perovskite solar cell provided in the embodiment of the present invention specifically includes the following steps:
(1) Fabrication of electron transport layer
TiO 2 A dense layer: and respectively carrying out ultrasonic treatment on the conductive glass (FTO) for 30min by using washing powder, deionized water, acetone and ethanol, and blow-drying the FTO from the side by using a clean nitrogen gun after cleaning. And (3) sticking a yellow adhesive tape on the conductive surface of the glass to reserve a reserved electrode, and then placing the substrate under an ozone cleaning machine for cleaning for 30min. Dripping about 2.2mL of titanium tetrachloride into 200mL of ice-water mixture dropwise, stirring and melting to obtain a clear and transparent solution, wherein the prepared TiCl 4 The solution concentration is 0.1M, which is used as cp-TiO 2 The precursor solution of (1). Then, the FTO treated by ozone is put into a clean glass culture dish, and the prepared TiCl is slowly poured into the FTO 4 Precursor solution, placing the sealed culture dish into a water bath kettle heated to 70 ℃, taking out after reacting for 2h, standing for 30min, cleaning with deionized water after cooling to room temperature, placing on a 150 ℃ hot bench for annealing for 2h, and annealing cp-TiO 2 And (5) finishing the manufacturing.
TiO 2 Manufacturing a nano array: firstly, preparing a mixture with a volume ratio (V: V) of 1:1, 100mL of deionized water mixed solution of hydrochloric acid, sealing tightly, placing on a magnetic stirrer, stirring at normal temperature for 30min, slowly dripping 1.5mL of tetra-n-butyl titanate solution after stirring, and stirring fully. Then the cp-TiO prepared in the above is added 2 Transferring the sample into a reaction kettle liner, placing the conductive glass surface upwards, pouring the stirred precursor solution, putting into the reaction kettle, heating at 150 ℃ for 105min in a drying box, taking out the sample after the reaction time is over, cleaning with deionized water, annealing at 150 ℃ for 2h in a muffle furnace 2 And completing the NA preparation.
SnO 2 Layer preparation: 1mL of tin tetrachloride was added to 200mL of deionized water and stirred until complete fusion. The preparation method is the same as that of TiO 2 A dense layer.
(2) Perovskite layer fabrication
Preparing a perovskite layer: weighing a certain amount of PbI 2 Dissolving powder in a mixed solvent of DMF and DMSO, and V: v =9:1, preparing PbI 2 The solution with concentration of 1.5M is placed on a magnetic stirrer and heated and stirred for 30min at 70 ℃; and (3) taking 6.39mg, 9mg and 90mg of iodomethylamine (MAI), chloromethylamine (MACl) and iodoformamidine (FAI) powder, adding 1mL of Isopropanol (IPA) solution into the mixed medicine powder, and continuously shaking on a shaking instrument for 15 min. The first step of the two-step spin coating method is to spin-coat PbI 2 Solution, using pipette gun to take 50 μ L of PbI 2 The solution was dropped onto the substrate surface after UV. The spin-coating time was 30s at 1500rpm and the plate was annealed for 10s at 70 ℃. Spin-coating organic salt solution, spin-coating 50 μ L organic salt on the sample, setting spin-coating parameters and spin-coating PbI 2 The technological parameters of the solution are consistent, and the solution is immediately taken down after the spin coating is finished and is placed on a constant-temperature heating table at 150 ℃ for annealing for 30min, so that the preparation of the PeSK film is finished.
And 2D layer preparation: and (3) spin-coating a PEAI solution on the prepared perovskite layer for post-treatment, wherein the concentration of the PEAI solution is 10mg/mL. The PEAI spin coating speed is 5000rpm, the acceleration is 9000rpm, and the time is 30s. And after the spin coating is finished, covering the glass slide on the upper surface to ensure that the perovskite is fully contacted with the PEAI solution, and annealing for 10min in a constant-temperature heating table at 100 ℃. After cooling to room temperature, the cover glass was removed.
(3) Electrode fabrication
C, manufacturing an electrode: and transferring the low-temperature carbon paste onto the 2D-3D layer by adopting a screen printing process. Immediately after the transfer process is finished, the steel plate is placed on a constant temperature heating table at 100 ℃ for annealing for 10min.
The above processes are all carried out in the air, the temperature is 25-28 ℃, and the humidity is 27-30%.
2. Application examples. In order to prove the creativity and the technical value of the technical scheme of the invention, the part is the application example of the technical scheme of the claims on specific products or related technologies.
The embodiment of the invention provides a preparation method of a 2D/3D perovskite solar cell electron transport layer, wherein the preparation method comprises a 3D perovskite layer and a 2D barrier layer, and the method comprises the following steps:
(1) Preparation of 3D perovskite layer on prepared electron transport layer
Weighing a certain amount of PbI 2 Dissolving powder in a mixed solvent of DMF and DMSO, and V: v =9:1, preparing PbI 2 The solution with concentration of 1.5M is placed on a magnetic stirrer and heated and stirred for 30min at 70 ℃; and (3) taking 6.39mg, 9mg and 90mg of iodomethylamine (MAI), chloromethylamine (MACl) and iodoformamidine (FAI) powder, adding 1mL of Isopropanol (IPA) solution into the mixed medicine powder, and continuously shaking on a shaking instrument for 15 min. The first step of the two-step spin coating method is to spin-coat PbI 2 Solution, using pipette gun to take 50 μ L of PbI 2 The solution was dropped onto the substrate surface after UV. The spin-coating time was 30s at 1500rpm and the plate was annealed for 10s at 70 ℃. Spin-coating organic salt solution, spin-coating 50 μ L organic salt on the sample, setting spin-coating parameters and spin-coating PbI 2 And the technological parameters of the solution are consistent, and the solution is immediately taken down after the spin coating is finished and is placed on a constant-temperature heating table at 150 ℃ for annealing for 30min, so that the preparation of the 3D perovskite film is finished.
(2) Preparation of 2D Barrier layer on 3D perovskite layer
And spin-coating PEAI solution on the prepared perovskite layer for post-treatment, wherein the concentration of the PEAI solution is 10mg/mL. The PEAI spin coating speed is 5000rpm, the acceleration is 9000rpm, and the time is 30s. And covering the glass slide on the upper surface after the spin coating is finished so that the perovskite is fully contacted with the PEAI solution, and annealing for 10min in a constant temperature heating table at 100 ℃. After cooling to room temperature, the cover glass was removed.
The concentration of the lead iodide solution used in step (1) was 1.5M
The mass ratio of the perovskite medicines used in the step (1) is MAI: MACl: FAI =6.39:9:90.
the PEAI concentration used in step (2) was 10mg/mL.
The embodiment of the invention provides a 2D/3D perovskite solar cell, which sequentially comprises an FTO transparent conductive glass substrate, an electron transmission layer, a perovskite layer, a 2D layer and a carbon electrode from bottom to top, wherein: the perovskite layer is a FAMA perovskite material, and the perovskite layer is the perovskite solar cell perovskite layer as defined in any one of claims 1 to 2. The 2D barrier layer is the 2D/3D perovskite solar cell 2D barrier layer of claim 3.
The thickness of the electron transport layer is 300nm.
The thickness of the perovskite layer is 600nm.
The thickness of the 2D layer is 30nm.
The thickness of the carbon electrode layer was 5 μm.
3. Evidence of the relevant effects of the examples. The embodiment of the invention achieves some positive effects in the process of research and development or use, and has great advantages compared with the prior art, and the following contents are described by combining data, diagrams and the like in the test process.
Example 1
The embodiment of the invention provides a 2D/3D perovskite solar cell which sequentially comprises FTO transparent conductive glass and TiO from bottom to top 2 The light absorption layer is formed on the substrate, the electron transmission layer is formed on the light absorption layer, the 2D layer is formed on the 2D layer, and the carbon electrode is formed on the carbon electrode. The absorption layer is made of perovskite material, and the 2D layer is PEAI. The manufacturing method comprises the following steps:
1. cleaning substrates
And respectively carrying out ultrasonic treatment on the conductive glass (FTO) for 30min by using washing powder, deionized water, acetone and ethanol, and blow-drying the FTO from the side by using a clean nitrogen gun after cleaning. And (3) sticking a yellow adhesive tape on the conductive surface of the glass to reserve a reserved electrode, and then placing the substrate under an ozone cleaning machine for cleaning for 30min.
2. Fabrication of an electron transport layer
(1)TiO 2 Dense layer
Dripping 2.2mL of titanium tetrachloride into 200mL of ice-water mixture dropwise, stirring for melting, and making the solution clear and transparent to obtain the TiCl 4 The solution concentration is 0.1M, which is used as cp-TiO 2 The precursor solution of (2). Then, the FTO treated by ozone is put into a clean glass culture dish, and the prepared TiCl is slowly poured into the FTO 4 Precursor solution, sealingPutting the good culture dish into a water bath kettle heated to 70 ℃, taking out after reacting for 2h, standing for 30min, cleaning with deionized water after cooling to room temperature, putting on a 150 ℃ hot bench for annealing for 2h, cp-TiO 2 And (5) finishing the manufacturing.
(2)TiO 2 Nano-array fabrication
Firstly, preparing a mixture with a volume ratio (V: V) of 1:1, stirring at normal temperature for 30min, dropwise adding 1.5mL of tetrabutyl titanate solution, and fully stirring. Then the cp-TiO prepared in the above is added 2 Transferring the sample into the inner container of a reaction kettle, pouring the stirred precursor solution, putting the mixture into the reaction kettle, heating the mixture in a drying box at 150 ℃ for 105min, taking out the sample after the reaction time is over, cleaning the sample with deionized water, annealing the sample in a muffle furnace at 150 ℃ for 2h 2 And completing the NA preparation.
(3)SnO 2 Layer fabrication
1mL of tin tetrachloride was added to 200mL of deionized water and stirred until complete fusion. The preparation method is the same as that of TiO 2 A dense layer.
3. Perovskite layer fabrication
Weighing a certain amount of PbI 2 Dissolving the powder in a mixed solvent of DMF and DMSO, and V: v =9:1, preparing PbI 2 The solution with concentration of 1.5M is placed on a magnetic stirrer and heated and stirred for 30min at 70 ℃; and (3) taking 6.39mg, 9mg and 90mg of iodomethylamine (MAI), chloromethylamine (MACl) and iodoformamidine (FAI) powder, adding 1mL of Isopropanol (IPA) solution into the mixed medicine powder, and continuously shaking on a shaking instrument for 15 min. Spin coating of PbI 2 Solution, using pipette gun to take 50 μ L of PbI 2 The solution was dropped onto the substrate surface after UV. The spin-coating time was 30s at 1500rpm and the plate was annealed for 10s at 70 ℃. Spin-coating organic salt solution, spin-coating 50 μ L organic salt on the sample, setting spin-coating parameters and spin-coating PbI 2 The technological parameters of the solution are consistent, and the solution is immediately taken down after the spin coating is finished and is placed on a constant-temperature heating platform at 150 ℃ for annealing for 30min, so that the preparation of the PeSK film is finished.
4. 2D layer fabrication
And spin-coating PEAI solution on the prepared perovskite layer for post-treatment, wherein the concentration of the PEAI solution is 10mg/mL. PEAI spin coating speed 5000rpm, acceleration 9000rpm, time 30s. And covering the glass slide on the upper surface after the spin coating is finished so that the perovskite is fully contacted with the PEAI solution, and annealing for 10min in a constant temperature heating table at 100 ℃. And cooling to room temperature and taking down the glass cover plate.
5. C electrode fabrication
And transferring the low-temperature carbon paste onto the 2D-3D layer by adopting a screen printing process. Immediately after the transfer process is finished, the steel plate is placed on a constant temperature heating table at 100 ℃ for annealing for 10min.
And completing the assembly of the 2D/3D perovskite solar cell.
And (4) respectively carrying out transmission spectrum, X-ray diffraction and field emission electron scanning microscope analysis on the perovskite thin film obtained by the 2D/3D preparation in the step (5). The instrument used for X-ray diffraction (XRD) analysis was D8 Advance, with the measurement conditions being 0.001 deg./step scan. The scanning electron microscope was operated at 20 KV.
In addition, the assembled 2D/3D perovskite solar cell is subjected to photoelectric property test. The current density-photovoltage (J-V) characteristics of the devices were measured from a computer controlled gishly 2400 source meter. The test was carried out in an ambient atmosphere simulating the irradiation of sunlight AM1.5G, at 100mW cm -2 Xenon lamp based solar simulator (from Newport co., ltd.). The External Quantum Efficiency (EQE) of the cell was measured by the DSP lock-in amplifier SR830 of the stanford research system model plus WDG3 monochrome kit and 500W xenon lamp. The intensity of each wavelength of light is calibrated to a standard single crystal silicon photovoltaic cell. The results of these tests are shown in the figures, respectively.
Fig. 2 is an SEM surface view of the perovskite thin film provided in the embodiment of the present invention, and it can be clearly seen from fig. 2 that the 2D/3D perovskite thin film has good crystallinity, flat surface, no obvious defect, and uniform 2D layer coverage, which is beneficial to the stability of the battery. The 3D perovskite surface morphology shows that the crystal grain size is different, the crystallization is not uniform, and the surface has defects and is not flat.
Fig. 3 is a structural diagram of a perovskite battery provided by an embodiment of the invention.
FIG. 4 is a UV-vis absorption spectrum of a 2D/3D perovskite layer, which may absorb more visible light than a 2D/3D perovskite thin film due to good crystallinity and flat surface of the perovskite thin film.
Fig. 5 is an XRD spectrum of the perovskite layer provided in the embodiments of the present invention, from which XRD peaks of 2D perovskite can be seen, demonstrating the presence of 2D perovskite. Fewer peaks in the XRD spectrum and no yellow phase perovskite peak appear, which proves that the perovskite thin film has good crystallinity.
FIG. 6 is a J-V curve for a 2D/3D perovskite cell provided by an embodiment of the invention. Wherein the open-circuit voltage, the short-circuit current, the filling factor and the photoelectric conversion efficiency are respectively as follows: 1.038V,24.54mA/cm 2 57.43% and 14.63%. J-V curves for 3D perovskite cells. Wherein the open-circuit voltage, the short-circuit current, the filling factor and the photoelectric conversion efficiency are respectively as follows: 1.02V,24.97mA/cm 2 48.68% and 12.45%.
Fig. 7 is a thermal stability diagram of a 2D/3D perovskite battery provided by an embodiment of the invention, and it can be seen that the efficiency of the 2D/3D perovskite battery can still reach 90% of the initial efficiency after being heated for 10 hours at 70 ℃ and at the ambient humidity of 33-35%. While the 3D perovskite thin film had dropped to below 80% of the initial efficiency at 6 h.
Fig. 8 is a stability chart of a 2D/3D perovskite battery provided by an embodiment of the invention, and it can be seen that the efficiency of the 2D/3D perovskite battery is still 90% of the initial efficiency after being placed under dry ambient conditions for 30 days, while the efficiency of the 3D perovskite battery is already reduced to 83% of the initial efficiency at day 7, and the efficiency is only 45% of the initial efficiency at day 30. Therefore, the stability of the 2D/3D perovskite battery is obviously improved.
Example 2
1. Cleaning substrates
And respectively carrying out ultrasonic treatment on the conductive glass (FTO) for 30min by using washing powder, deionized water, acetone and ethanol, and blow-drying the FTO from the side by using a clean nitrogen gun after cleaning. And (3) sticking a yellow adhesive tape on the conductive surface of the glass to reserve a reserved electrode, and then placing the substrate under an ozone cleaning machine for cleaning for 30min.
2. Fabrication of an electron transport layer
(1)TiO 2 Is denseLayer(s)
Dripping 2.2mL of titanium tetrachloride into 200mL of ice-water mixture dropwise, stirring for melting, and making the solution clear and transparent to obtain the TiCl 4 The concentration of the solution was 0.1M, which was used as cp-TiO 2 The precursor solution of (2). Then, the FTO treated by ozone is put into a clean glass culture dish, and the prepared TiCl is slowly poured into the FTO 4 Precursor solution, placing sealed culture dish in water bath kettle heated to 70 deg.C, reacting for 2 hr, taking out, standing for 30min, cooling to room temperature, cleaning with deionized water, annealing at 150 deg.C for 2h, and annealing with cp-TiO 2 And (5) finishing the manufacturing.
(2)TiO 2 Nano-array fabrication
Firstly, preparing a mixture with a volume ratio (V: V) of 1:1, stirring at normal temperature for 30min, dropwise adding 1.5mL of tetrabutyl titanate solution, and fully stirring. Then the cp-TiO prepared in the above is added 2 Transferring the sample into the inner container of a reaction kettle, pouring the stirred precursor solution, putting the stirred precursor solution into the reaction kettle, heating the sample in a drying box at 150 ℃ for 105min, taking out the sample after the reaction time is over, cleaning the sample with deionized water, annealing the sample in a muffle furnace at 150 ℃ for 2h 2 And completing the NA preparation.
(3)SnO 2 Layer fabrication
1mL of tin tetrachloride was added to 200mL of deionized water and stirred until complete fusion. The preparation method is the same as that of TiO 2 A dense layer.
3. Perovskite layer fabrication
Weighing a certain amount of PbI 2 Dissolving the powder in a mixed solvent of DMF and DMSO, and V: v =9:1, preparing PbI 2 The solution with concentration of 1.5M is placed on a magnetic stirrer and heated and stirred for 30min at 70 ℃; and (3) taking 6.39mg, 9mg and 90mg of iodomethylamine (MAI), chloromethylamine (MACl) and iodoformamidine (FAI) powder, adding 1mL of Isopropanol (IPA) solution into the mixed medicine powder, and continuously shaking on a shaking instrument for 15 min. Spin coating of PbI 2 Solution, using pipette gun to take 50 μ L of PbI 2 The solution is dropped on the surface of the substrate after UV. The spin-coating time was 30s at 1500rpm and the plate was annealed for 10s at 70 ℃. Spin coating organic salt solution, collecting 50 μ L organic solutionSalt spin coating on sample, spin coating parameter setting and spin coating PbI 2 The technological parameters of the solution are consistent, and the solution is immediately taken down after the spin coating is finished and is placed on a constant-temperature heating table at 150 ℃ for annealing for 30min, so that the preparation of the PeSK film is finished.
4. 2D layer fabrication
And spin-coating PEAI solution on the prepared perovskite layer for post-treatment, wherein the concentration of the PEAI solution is 5mg/mL. The PEAI spin coating speed is 5000rpm, the acceleration is 9000rpm, and the time is 30s. And covering the glass slide on the upper surface after the spin coating is finished so that the perovskite is fully contacted with the PEAI solution, and annealing for 10min in a constant temperature heating table at 100 ℃. After cooling to room temperature, the cover glass was removed.
5. C electrode fabrication
And transferring the low-temperature carbon paste onto the 2D-3D layer by adopting a screen printing process. Immediately after the transfer process is finished, the steel plate is placed on a constant temperature heating table at 100 ℃ for annealing for 10min.
Example of the invention J-V curve of 2D/3D perovskite cell. Wherein the open circuit voltage, the short circuit current, the fill factor and the photoelectric conversion efficiency are respectively as follows: 1.029V,24.69mA/cm 2 51.93% and 13.46%. The absorption value of the UV-vis absorption spectrum is slightly lower than that of the example 1, and the results of SEM and XRD have no obvious difference.
Example 3
1. Cleaning substrates
And respectively carrying out ultrasonic treatment on the conductive glass (FTO) for 30min by using washing powder, deionized water, acetone and ethanol, and blow-drying the FTO from the side by using a clean nitrogen gun after cleaning. And (3) sticking a yellow adhesive tape on the conductive surface of the glass to reserve a reserved electrode, and then placing the substrate under an ozone cleaning machine for cleaning for 30min.
2. Fabrication of an electron transport layer
(1)TiO 2 Dense layer
Dripping 2.2mL of titanium tetrachloride into 200mL of ice-water mixture dropwise, stirring for melting, and making the solution clear and transparent to obtain the TiCl 4 The concentration of the solution was 0.1M, which was used as cp-TiO 2 The precursor solution of (2). Then, the FTO treated by ozone is put into a clean glass culture dish, and the prepared TiCl is slowly poured into the FTO 4 Precursor solution, sealingPlacing the culture dish into a water bath kettle heated to 70 deg.C, reacting for 2 hr, taking out, standing for 30min, cooling to room temperature, cleaning with deionized water, annealing at 150 deg.C for 2h, and annealing with cp-TiO 2 And (5) finishing the manufacturing.
(2)TiO 2 Nano-array fabrication
Firstly, preparing a mixture with a volume ratio (V: V) of 1:1, stirring at normal temperature for 30min, dropwise adding 1.5mL of tetra-n-butyl titanate solution, and fully stirring. Then the cp-TiO prepared in the above is added 2 Transferring the sample into the inner container of a reaction kettle, pouring the stirred precursor solution, putting the stirred precursor solution into the reaction kettle, heating the sample in a drying box at 150 ℃ for 105min, taking out the sample after the reaction time is over, cleaning the sample with deionized water, annealing the sample in a muffle furnace at 150 ℃ for 2h 2 And completing the NA preparation.
(3)SnO 2 Layer fabrication
1mL of tin tetrachloride was added to 200mL of deionized water and stirred until complete fusion. The preparation method is the same as that of TiO 2 A dense layer.
3. Perovskite layer fabrication
Weighing a certain amount of PbI 2 Dissolving powder in a mixed solvent of DMF and DMSO, and V: v =9:1, preparing PbI 2 The solution with concentration of 1.5M is placed on a magnetic stirrer and heated and stirred for 30min at 70 ℃; and (3) taking 6.39mg, 9mg and 90mg of iodomethylamine (MAI), chloromethylamine (MACl) and iodoformamidine (FAI) powder, adding 1mL of Isopropanol (IPA) solution into the mixed medicine powder, and placing on a shaker for continuously shaking for 15 min. Spin coating of PbI 2 Solution, using pipette gun to take 50 μ L of PbI 2 The solution was dropped onto the substrate surface after UV. The spin-coating time was 30s at 1500rpm and the plate was annealed for 10s at 70 ℃. Spin-coating organic salt solution, spin-coating 50 μ L organic salt on the sample, setting spin-coating parameters and spin-coating PbI 2 The technological parameters of the solution are consistent, and the solution is immediately taken down after the spin coating is finished and is placed on a constant-temperature heating platform at 150 ℃ for annealing for 30min, so that the preparation of the PeSK film is finished.
4. 2D layer fabrication
And spin-coating PEAI solution on the prepared perovskite layer for post-treatment, wherein the concentration of the PEAI solution is 10mg/mL. PEAI spin coating speed 4000rpm, acceleration 9000rpm, time 30s. And covering the glass slide on the upper surface after the spin coating is finished so that the perovskite is fully contacted with the PEAI solution, and annealing for 10min in a constant temperature heating table at 100 ℃. After cooling to room temperature, the cover glass was removed.
5. C electrode fabrication
And transferring the low-temperature carbon paste onto the 2D-3D layer by adopting a screen printing process. Immediately after the transfer process is finished, the steel plate is placed on a constant temperature heating table at 100 ℃ for annealing for 10min.
Example of the invention J-V curve for 2D/3D perovskite cells. Wherein the open-circuit voltage, the short-circuit current, the filling factor and the photoelectric conversion efficiency are respectively as follows: 1.024V,24.89mA/cm 2 55.93% and 14.26%. The absorption spectrum was similar to that of example 1.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of a 2D/3D perovskite solar cell is characterized by comprising the following steps:
and (2) adding a glass slide on the surface of the 2D perovskite layer to ensure that a PEAI solution is fully contacted with the surface of the 3D perovskite, using PEAI as a 2D perovskite barrier layer, growing a 2D covering layer on the top of the 3D perovskite film in situ, improving the annealing method of the 2D layer and the PEAI concentration, and using low-temperature carbon slurry to replace a hole transport layer HTM and a metal electrode, thereby preparing the 2D/3D perovskite solar cell.
2. The method of fabricating a 2D/3D perovskite solar cell as defined in claim 1, wherein the method of fabricating a 2D/3D perovskite solar cell comprises the steps of:
step one, manufacturing an electron transport layer comprising TiO 2 Dense layer, tiO 2 Nanoarrays and SnO 2 Layer manufacturing;
step two, respectively manufacturing a perovskite layer and a 2D layer;
and step three, manufacturing the C electrode by adopting a screen printing process.
3. The method of making a 2D/3D perovskite solar cell of claim 2, wherein the TiO in step one 2 The preparation of the compact layer comprises the following steps:
respectively carrying out ultrasonic treatment on the conductive glass FTO for 30min by using washing powder, deionized water, acetone and ethanol, and blow-drying the FTO from the side by using a clean nitrogen gun after cleaning is finished; after a yellow adhesive tape is pasted on the conductive surface of the glass to reserve a reserved electrode, placing the substrate under an ozone cleaning machine, and cleaning for 30min; dropwise adding 2.2mL of titanium tetrachloride into 200mL of ice-water mixture, stirring and melting, wherein the solution is clear and transparent, and the prepared TiCl 4 The concentration of the solution is 0.1M to obtain the cp-TiO 2 The precursor solution of (2); placing the FTO treated by ozone into a clean glass culture dish, and slowly pouring the prepared TiCl 4 Precursor solution, putting the sealed culture dish into a water bath kettle heated to 70 ℃, taking out after reacting for 2h, and standing for 30min; after cooling to room temperature, cleaning with deionized water, placing on a 150 ℃ hot bench for annealing for 2h 2 And finishing the sample preparation.
4. The method of making a 2D/3D perovskite solar cell of claim 2, wherein the TiO in step one 2 The preparation of the nano array comprises the following steps:
preparing a mixture with a volume ratio of 1:1, 100mL of hydrochloric acid deionized water mixed solution, sealing and tightly arranging the mixed solution, placing the mixed solution on a magnetic stirrer, stirring the mixed solution at normal temperature for 30min, slowly dripping 1.5mL of tetrabutyl titanate solution after stirring, and fully stirring to obtain a precursor solution; the prepared cp-TiO 2 Transferring the sample into a liner of a reaction kettle, placing the conductive glass surface upwards, pouring the stirred precursor solution into the reaction kettle, and heating the mixture in a drying oven at 150 ℃ for 105min; after the reaction time is over, taking out the sample, washing the sample by deionized water, and placing the sample in a muffle furnaceAnnealing at the temperature of 150 ℃ for 2h and TiO 2 And completing the NA preparation.
5. The method of preparing a 2D/3D perovskite solar cell as claimed in claim 2, wherein the SnO in step one 2 The layer fabrication includes:
1mL of stannic chloride is put into 200mL of deionized water and stirred until the stannic chloride is completely fused, and the preparation method is the same as that of TiO 2 A dense layer.
6. The method of fabricating a 2D/3D perovskite solar cell as claimed in claim 2, wherein the fabrication of the perovskite layer in the second step comprises:
weighing a certain amount of PbI 2 Dissolving the powder in a mixed solvent of DMF and DMSO, and V: v =9:1, preparing PbI 2 The solution with concentration of 1.5M is placed on a magnetic stirrer and heated and stirred for 30min at 70 ℃; respectively taking 6.39mg, 9mg and 90mg of iodomethylamine, chloromethane and iodoformamidine powder, adding 1mL of isopropanol solution into the mixed medicine powder, and continuously shaking on a shaking instrument for 15min; the first step of the two-step spin coating method is to spin coat PbI 2 Solution, using pipette gun to take 50 μ L of PbI 2 Dropping the solution on the surface of the substrate after UV; the spin coating time is 30s at the spin coating speed of 1500rpm, and the annealing is carried out for 10s on a hot bench at the temperature of 70 ℃; spin-coating an organic salt solution, taking 50 mu L of organic salt to spin-coat on a sample, wherein the spin-coating rotation speed is 1500rpm, and the spin-coating time is 30s; and immediately taking down the film after the spin coating, placing the film on a constant-temperature heating table at 150 ℃ for annealing for 30min, and finishing the preparation of the PeSK film.
7. The method of fabricating a 2D/3D perovskite solar cell as claimed in claim 2, wherein the fabrication of the 2D layer in step two comprises:
spin-coating PEAI solution on the prepared perovskite layer for post-treatment, wherein the concentration of the PEAI solution is 10mg/mL; the PEAI spin-coating rotation speed is 5000rpm, the acceleration is 9000rpm, and the time is 30s; covering the glass slide on the upper surface after the spin coating is finished so that the perovskite is fully contacted with the PEAI solution, and placing the glass slide on a constant temperature heating table at 100 ℃ for annealing for 10min; and cooling to room temperature and taking down the glass cover plate.
8. The method for preparing a 2D/3D perovskite solar cell according to claim 2, wherein the C electrode in step three comprises:
and transferring the low-temperature carbon slurry onto the 2D-3D layer by adopting a screen printing process, and immediately annealing for 10min on a constant-temperature heating table at 100 ℃ after the transfer process is finished.
9. The method of claim 1, wherein the 2D/3D perovskite solar cell is fabricated in air at a temperature of 25-28 ℃ and a humidity of 27-30%.
10. A 2D/3D perovskite solar cell prepared by carrying out the method for preparing a 2D/3D perovskite solar cell according to any one of claims 1 to 9.
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