CN115172612A - Method for improving flexibility and mechanical property of flexible perovskite solar cell - Google Patents
Method for improving flexibility and mechanical property of flexible perovskite solar cell Download PDFInfo
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Abstract
A method for improving flexibility and mechanical property of a flexible perovskite solar cell comprises the following steps of when a conductive substrate is defined as the lowest layer: a conductive substrate layer; an electron transport layer; a polymer and inorganic metal oxide nanoparticle modified perovskite light absorbing layer; a hole transport layer; a counter electrode; the polymer is one or more of chitosan, polyethylene oxide, polyacrylonitrile, polymethyl methacrylate and poly (vinylidene fluoride-co-hexafluoropropylene); the inorganic metal nano oxide is TiO 2 、ZnO、Al 2 O 3 、SiO 2 And ZrO 2 One or more of them. The invention adapts to the perovskite layerThe bulk phase doping of the polymer and the inorganic metal nano oxide nanoparticles is realized, the flexibility and the environmental stability of the device are improved, the ion migration in the perovskite film is inhibited, the perovskite crystal is stabilized, and the effect of releasing stress is realized.
Description
Technical Field
The invention relates to a method for improving the performance of a flexible perovskite solar cell, in particular to a method for improving the flexibility and the mechanical performance of the flexible perovskite solar cell.
Background
The metal perovskite is an ideal material for constructing the flexible solar cell due to the advantages of unique optical and physical properties, low cost, capability of being prepared by low-temperature solution and the like. Under the support of technologies such as composite engineering, surface passivation, interface modification and manufacturing process optimization, the photoelectric conversion efficiency of flexible perovskite solar cells (F-PSCs) exceeds 21% by combining the research and development of a low-temperature charge transmission layer, a perovskite light absorption layer and a flexible conductive substrate. These excellent results demonstrate the enormous potential of F-PSCs in wearable and portable electronic devices, curved electronic displays, and the like. However, the efficiency, stability and film quality of F-PSCs in large area printing are still the bottlenecks that limit their commercial applications.
Research in the field of F-PSCs has progressed rapidly since its first appearance, and many developments in rigid PSCs have been replicated in F-PSCs. However, there are still a number of important factors that limit further improvements in the efficiency of F-PSCs. For example, the difficulty in preparing high quality low temperature electron transport layers, the increased resistance of the plastic substrate due to thermal deformation during annealing, the charge carrier loss at the interface between the electrode and the charge transport layer, the poor surface roughness of the plastic substrate, the poor morphology of the top layer including the electron transport layer and the perovskite layer, the low transmittance of the plastic substrate in the uv and visible ranges, and the like, can essentially make the efficiency of flexible devices still lag that of rigid devices.
With the increasing efficiency of F-PSCs, environmental stability, flexibility, and stretchability of devices are becoming more of a concern. Therefore, how to improve the stability of F-PSCs to meet various wearable and portable electronic devices becomes a major challenge in today's society. Researchers are constantly shifting the center of gravity toward stability. It was found that the perovskite layer, the organic electron transport layer and the hole transport layer were accelerated in the presence of air, moisture and heat cycling. The degradation and phase transition of perovskite crystals are mainly due to its ionic nature, oxygen, moisture, ultraviolet radiation and heat being the main factors of perovskite crystal degradation, however the degradation mechanism of perovskite layers is not fully understood. In addition, polymeric substrates have a poor barrier to moisture and oxygen ingress, and water and oxygen transmission through flexible substrates can cause further degradation of the perovskite and other constituent layers. Thus, F-PSCs present serious long-term environmental stability problems. Improving the stability of F-PSCs requires consideration of numerous factors, such as the composition of the perovskite, the uniformity and crystallinity of the perovskite thin film, interface engineering, choice of charge transport materials and electrodes, and packaging techniques. In addition, bending stability is one of the important factors to be solved for commercial application of F-PSCs, and is mainly limited by the mechanical strength of the transparent electrode and the adhesion property between the charge transport layer and the perovskite thin film. Conventional highly efficient flexible perovskite devices are fabricated on ITO/PET or PEN substrates, and the rigid nature of ITO can lead to cracking of the film after repeated bending, resulting in leakage of current carriers and increased series resistance, which can render the device ineffective.
CN 107104189A discloses a perovskite thin-film solar cell, which comprises a cathode, a perovskite light absorption layer and an anode, wherein an electrode interface modification layer is further disposed between the anode and the perovskite light absorption layer, the electrode interface modification layer contains atoms and/or ions capable of reacting with the perovskite light absorption layer to promote the crystallinity of perovskite crystals, and the electrode interface modification layer is further used for improving the surface roughness and morphology of the anode. The battery uses oxide particles and polymers as an interface modification layer on the upper interface of the perovskite to improve the humidity stability of the device, does not mention how to improve the stability of the perovskite light absorption layer, lacks research on the bending stability of a flexible device, and has low photoelectric conversion efficiency of the obtained device.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art and provide a method for improving the flexibility and mechanical properties of a flexible perovskite solar cell.
The technical scheme adopted by the invention for solving the technical problem is as follows: a method for improving flexibility and mechanical properties of a flexible perovskite solar cell is characterized in that when a conductive substrate is defined as the lowest layer, the solar cell sequentially comprises the following steps from bottom to top: a conductive substrate layer; an electron transport layer; a polymer and inorganic metal oxide nanoparticle modified perovskite light absorbing layer; a hole transport layer; a counter electrode.
Preferably, the conductive substrate layer is a transparent polyethylene naphthalate flexible substrate (ITO-PEN).
Preferably, the electron transport layer is SnO 2 、TiO 2 ZnO or PCBM electron transport layer.
Preferably, the polymer is one or more of chitosan, polyethylene oxide (PEO), polyacrylonitrile (PAN), polymethyl methacrylate (PMMA), polyvinylidene fluoride (PVDF-HFP); the inorganic metal nano oxide is TiO 2 、ZnO、Al 2 O 3 、SiO 2 And ZrO 2 One or more of them.
Preferably, the perovskite light absorption layer is ABX 3 Perovskite light-absorbing layer, wherein A is CH 3 NH 3 Or Cs, B is Pb, sn, in or Ge, and X is one or more of I, br or Cl.
Preferably, the hole transport material is a small molecule polymer, more preferably one or more of Spiro-OMeTAD, PSS, P3HT, PEDOT and NiO, and further preferably Spiro-OMeTAD and/or P3HT.
Preferably, the method for improving the flexibility and the mechanical property of the flexible perovskite solar cell specifically comprises the following steps:
(1) Cleaning the transparent ITO-PEN to prepare a transparent conductive substrate;
(2) Preparing an electron transport layer on the surface of the prepared conductive substrate;
(3) Preparing polymer and inorganic metal oxide nanoparticle modified perovskite ABX on the surface of the prepared electron transport layer 3 A light absorbing layer;
(4) Perovskite ABX modified in prepared polymer and inorganic metal oxide nanoparticles 3 Preparing a hole transport layer on the surface of the light absorption layer;
(5) And (3) evaporating a thin metal counter electrode on the surface of the prepared hole transport layer.
More preferably, in the step (1), the cleaning mode is as follows: and (2) placing the transparent ITO-PEN conductive glass in deionized water, absolute ethyl alcohol and isopropanol, respectively, ultrasonically oscillating for 10-20 min, baking for 10-25 min at 80-120 ℃ (for removing visible impurities on the surface), and treating for 20-30 min by ultraviolet ozone (for removing organic groups on the surface to reduce the water contact angle).
More preferably, in the step (2), the electron transport layer is prepared by the following steps: and (3) dropwise adding the electronic transmission material dispersion liquid on the surface of the conductive substrate, spin-coating at 4000-6000 rpm for 20-40 s (uniformly forming a film), and heating at 150-200 ℃ for 30-40 min to obtain the conductive substrate.
Further preferably, in the step (2), the electron transport material dispersion is made of an electron transport material (SnO) 2 、TiO 2 ZnO or PCBM) with a solvent (deionized water or isopropanol or chlorobenzene)) in a volume ratio of 1: mixing 1 to 8, and performing ultrasonic dispersion to prepare the material.
More preferably, in the step (3), the perovskite precursor solution after filtration is dripped on the surface of the electron transport layer, and the perovskite ABX modified by polymer and inorganic metal oxide nanoparticles is obtained by spin coating, heat treatment and annealing 3 A light absorbing layer.
More preferably, in the step (3), the preparation method of the polymer and inorganic metal oxide nanoparticle modified perovskite precursor solution comprises the following steps: mixing polymer, inorganic oxide nanoparticles, AX and BX 2 Dissolving the mixture in dimethyl sulfoxide (DMSO) or a solution of the mixture and N, N-Dimethylformamide (DMF), and heating and stirring the mixture for 4 to 12 hours at the temperature of 65 to 75 ℃.
More preferably, in the step (3), in the perovskite precursor liquid, the addition amount of the polymer is 0 to 10 percent of the total mass of the precursor liquid, the addition amount of the inorganic metal oxide nanoparticles is 0 to 10 percent of the total mass of the precursor liquid, the addition amount of the AX is 10 to 20 percent of the total mass of the precursor liquid, and the BX is 2 The addition amount of the compound is 20 to 30 percent of the total mass of the precursor liquid, and the addition amount of the dimethyl sulfoxide is equivalent to the addition amount of the dimethyl sulfoxideThe total mass of the precursor solution is 20-60%, and the addition amount of the N, N-dimethylformamide is 0-50% of the total mass of the precursor solution.
More preferably, in the step (3), the diameter of the filter head used for filtering is 0.22 to 0.45
。
More preferably, in the step (3), the rotation speed of the spin coating is 3500 to 7500 rpm, and the time is 20 to 40 s.
More preferably, in the step (3), 200-300 times of the countdown is added when the spin coating is carried out for 10-24 s
Ethyl acetate or chlorobenzene solution, (to aid rapid crystallization of the perovskite).
More preferably, in the step (3), the temperature of the heat treatment is 70 to 110 ℃, and the time is 10 to 20 min; by the heat treatment in the mode, the smooth perovskite film is obtained by annealing.
More preferably, in the step (4), the hole transport solution is dropwise added to the surface of the polymer and inorganic metal oxide nanoparticle modified perovskite light absorption layer, and spin coating is performed to obtain the hole transport layer.
Further preferably, in the step (4), in the hole transport solution, the mass of lithium bistrifluoromethane sulfonimide is 0.2 to 2% of the total mass of the solution, the mass of 4-tert-butylpyridine is 0.8 to 3% of the total mass of the solution, the mass of chlorobenzene is 60 to 80% of the total mass of the solution, and the mass of the hole transport material is 10 to 30% of the total mass of the solution.
More preferably, in the step (4), the rotation speed of the spin coating is 2000 to 3500 rpm, and the time is 30 to 40 s.
More preferably, in step (5), a thin metal counter electrode is evaporated by vacuum evaporation.
More preferably, in the step (5), the vacuum evaporation rate is 0.1 to 0.6 nm/s, and the thickness of the thin metal counter electrode is 10 to 60 nm.
Further preferably, the metal is plated with gold or silver.
The invention provides a method for improving the flexibility and mechanical property of flexible perovskite solar energy, which is characterized in that a perovskite layer is doped with a proper amount of polymer and inorganic metal nano oxide nanoparticles, and the polymer can fill gaps of a perovskite film in the crystallization process, so that perovskite crystal grains are more compact, and the generation of defects and traps is reduced; the flexible device can damage the perovskite thin film in the bending process to cause the deformation of a crystal structure, and the polymer with good flexibility can be used as a plasticizer of the perovskite thin film to form a cross-linked network structure around perovskite crystal grains, so that the internal cracking capability of the perovskite thin film can be reduced, the hydrophobicity of the perovskite thin film can be enhanced, and the flexibility and the environmental stability of the flexible device can be further improved; in addition, on the basis of polymer doping, an inorganic metal nano oxide nano particle doped perovskite light absorption layer is added, the surface activity of the inorganic metal oxide nano particle is very large, the surface of the inorganic metal oxide nano particle contains rich hydroxyl, and the inorganic metal oxide nano particle can be used as a rigid framework to form hydrogen bond connection with each component in a polymer matrix, so that the mechanical property and the bending stability of the flexible device are further improved together. Generally, the invention provides theoretical and technical basis for improving the flexibility and mechanical property of the flexible perovskite solar cell.
Compared with the prior art, the invention has the beneficial effects that:
(1) The perovskite layer is doped with a proper amount of polymer and inorganic metal nano oxide nanoparticles, the crystals of the polymer are used for filling the defects of perovskite crystal grains, and the toughness of the polymer and the formation of a cross-linked network structure between perovskites are used for enhancing the flexibility and the environmental stability of the device; the surface of the inorganic oxide nano particle is provided with hydroxyl, and the hydroxyl can form a complex with polymer molecules, so that the perovskite can be prevented from being corroded by water and oxygen, the ion migration in the perovskite film can be further inhibited, and in addition, the crystallinity of the polymer molecules of the agar can be reduced by the inorganic oxide nano particle, so that the perovskite crystal can be stabilized, and the effect of releasing stress is achieved;
(2) According to the invention, the perovskite light absorption layer is modified by co-doping of the polymer and the inorganic oxide nanoparticles, so that the quality of the perovskite film is improved, the contact of each functional layer is improved, the charge recombination rate is reduced, and the charge transmission capability is enhanced;
(3) The invention can evaporate ultrathin metal counter electrodes, reduce the device cost, and construct the flexible perovskite solar cell to achieve the effect of double-sided photoresponse.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specified, the reagents and materials used in the present invention are commercially available products or products obtained by a known method.
Example 1
This example uses polymer (chitosan) and inorganic nano-oxide nanoparticles (TiO) 2 ) The embodiment is based on a method for improving the flexibility and mechanical property of a flexible perovskite solar cell, and when the conductive substrate is defined as the lowest layer, the embodiment sequentially comprises the following steps from bottom to top: a transparent ITO-PEN conductive substrate; a tin dioxide electron transport layer; with chitosan (polymer) and TiO 2 (inorganic oxide nanoparticles) modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 A light absorbing layer; a hole transport layer; a gold counter electrode.
The embodiment is based on a method for improving the flexibility and mechanical properties of a flexible perovskite solar cell, and the preparation method comprises the following steps:
(1) Cleaning transparent ITO-PEN to obtain a transparent conductive substrate: respectively adopting deionized water, absolute ethyl alcohol and isopropanol to ultrasonically vibrate for 10 min to clean the ITO-PEN conductive substrate, putting the ITO-PEN conductive substrate into an oven to be dried for 15 min at 100 ℃ after ultrasonic treatment to remove visible impurities on the surface, and then treating the ITO-PEN conductive substrate on an ultraviolet ozone processor for 25 min to remove organic groups on the surface so as to reduce a water contact angle;
(2) Preparing a tin dioxide electron transport layer on the surface of the transparent conductive substrate obtained in the step (1): dropwise adding tin dioxide colloid dispersion liquid on the transparent conductive substrate after ozone treatment, uniformly forming a film by spin coating at 5000 rpm for 20 s, and heating at 160 ℃ for 35 min on a heating table to obtain a tin dioxide electronic transmission layer, wherein the tin dioxide colloid dispersion liquid is prepared by mixing tin dioxide colloid and deionized water according to a volume ratio of 1:4, mixing and ultrasonically dispersing;
(3) Preparing chitosan and TiO on the surface of the stannic oxide electron transport layer obtained in the step (2) 2 Modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 A light absorbing layer;
(3-I) mixing chitosan and TiO 2 The molar ratio is 1:1 CH 3 NH 3 I and PbI 2 Dissolved in a solvent with the volume ratio of 1:4, heating and stirring the mixture solution of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF) at the temperature of 60 ℃ for 12 hours to obtain chitosan and TiO 2 The modified organic-inorganic hybrid perovskite precursor solution comprises 1 percent of chitosan and TiO 2 Is added in an amount of 2% of the total mass, CH 3 NH 3 The amount of I added is 15% of the total mass, pbI 2 The amount of the added DMSO solvent is 22% of the total mass, the amount of the added DMSO solvent is 13% of the total mass, and the amount of the added DMF solvent is 50% of the total mass;
(3-II) mixing the chitosan obtained in the step (3-I) and TiO 2 Filtering the modified organic-inorganic hybrid perovskite precursor solution by a filter head with the diameter of 0.22 mu m, dripping the modified organic-inorganic hybrid perovskite precursor solution on the stannic oxide electronic transmission layer obtained in the step (2), and obtaining chitosan and TiO in a spin coating mode 2 Modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 A light absorption layer, wherein the spin coating process is set to be 5000 rpm for 30s; adding 250 mu L of ethyl acetate solution when the solution is poured for 23 s by spin coating, carrying out heat treatment at 100 ℃ for 10 min, and annealing to obtain a smooth perovskite film;
(4) The organic-inorganic hybrid perovskite CH obtained in the step (3) 3 NH 3 PbI 3 Preparing a hole transport layer on the surface of the light absorbing layer: adding lithium bis (trifluoromethanesulfonylimide) in a hole transport solution in an amount which accounts for 1.5% of the total solution mass, adding 4-tert-butylpyridine in an amount which accounts for 2.5% of the total solution mass, adding chlorobenzene in an amount which accounts for 66% of the total solution mass, adding P3HT (hole transport material) in an amount which accounts for 30% of the total solution mass, and dropwise adding the P3HT solution into the organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 Obtaining a hole transport layer on the surface of the light absorption layer in a spin coating mode, setting a spin coating process at 3000 rpm for 30s;
(5) And evaporating a thin metal counter electrode on the surface of the hole transport layer: vacuum evaporating 40 nm gold counter electrode at 0.4 nm/s rate by vacuum evaporation method.
The performance of the translucent flexible organic-inorganic hybrid perovskite solar cell based on polymer and inorganic oxide nanoparticles obtained in this example was tested: in the room temperature environment, the humidity is more than 50 percent, a xenon lamp is used for simulating sunlight, and the light intensity is 100 mW/cm 2 The effective illumination area is 0.25 cm 2 The photoelectric conversion efficiency of the solar cell is 22%, after the solar cell is placed for 290 days under the condition of no packaging, the photoelectric efficiency is reduced to 97% of the initial value, and 95% of the initial efficiency can be still maintained after the solar cell is circularly bent 3000 times (the bending radius is 3 mm).
Example 2
This example, which is based on a method for improving the flexibility and mechanical properties of a flexible perovskite solar cell, uses a Polymer (PEO) and inorganic nano-oxide nanoparticles (ZnO) to modify a perovskite layer, and defines a conductive substrate as the lowermost layer, and includes, in order from bottom to top: a transparent ITO-PEN conductive substrate; a tin dioxide electron transport layer; organic-inorganic hybrid perovskite CH modified with PEO (polymer) and ZnO (inorganic oxide nanoparticles) 3 NH 3 SnClI 2 A light absorbing layer; a hole transport layer; a gold counter electrode.
The preparation method of the semitransparent flexible organic-inorganic hybrid perovskite solar cell based on the polymer and the inorganic oxide nanoparticles comprises the following steps:
(1) Cleaning transparent ITO-PEN to obtain a transparent conductive substrate: respectively adopting deionized water, absolute ethyl alcohol and isopropanol to ultrasonically vibrate for 15 min to clean the ITO-PEN conductive substrate, putting the ITO-PEN conductive substrate into an oven to be dried for 15 min at 80 ℃ after ultrasonic treatment to remove visible impurities on the surface, and then treating the ITO-PEN conductive substrate on an ultraviolet ozone processor for 30 min to remove organic groups on the surface so as to reduce a water contact angle;
(2) Preparing a tin dioxide electron transport layer on the surface of the transparent conductive substrate obtained in the step (1): dropwise adding tin dioxide colloid dispersion liquid on the transparent conductive substrate after ozone treatment, carrying out spin coating for 30s at 4000 rpm by a spin coating method to uniformly form a film, heating for 30 min at 150 ℃ on a heating table to obtain a tin dioxide electronic transmission layer, wherein the tin dioxide colloid dispersion liquid is prepared by mixing tin dioxide colloid and deionized water according to a volume ratio of 1:1, mixing and ultrasonically dispersing;
(3) Preparing PEO and ZnO modified organic-inorganic hybrid perovskite CH on the surface of the stannic oxide electron transport layer obtained in the step (2) 3 NH 3 SnClI 2 A light absorbing layer;
(3-I) mixing PEO, znO and a mixture of PEO and ZnO in a molar ratio of 1:1 CH 3 NH 3 Cl and SnI 2 Dissolving in a solvent with the volume ratio of 2:1, heating and stirring for 4 hours at 65 ℃ in a mixed solution of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF) to obtain a PEO and ZnO modified organic-inorganic hybrid perovskite precursor solution, wherein the addition of the PEO is 2 percent of the total mass, the addition of the ZnO is 2 percent of the total mass, and the addition of the CH is 3 NH 3 The amount of Cl added corresponds to 15% of the total mass, snI 2 The addition amount of (2) is equal to 15% of the total mass, the addition amount of the DMSO solvent is equal to 60% of the total mass, and the addition amount of the DMF solvent is equal to 6% of the total mass;
(3-II) filtering the PEO and ZnO modified organic-inorganic hybrid perovskite precursor solution obtained in the step (3-I) through a filter head with the diameter of 0.22 mu m, then dropwise adding the filtered PEO and ZnO modified organic-inorganic hybrid perovskite precursor solution on the tin dioxide electron transport layer obtained in the step (2), and obtaining the PEO and ZnO modified organic-inorganic hybrid perovskite CH in a spin coating mode 3 NH 3 SnClI 2 Light absorbing layer provided with a spinThe coating process is 5500 rpm,35 s; adding 200 mu L of chlorobenzene solution when the solution is poured for 25 s by spin coating, carrying out heat treatment for 10 min at 105 ℃, and annealing to obtain a smooth perovskite film;
(4) PEO and ZnO modified organic-inorganic hybrid perovskite CH obtained in step (3) 3 NH 3 SnClI 2 Preparing a hole transport layer on the surface of the light absorbing layer: adding lithium bis (trifluoromethanesulfonyl) imide in the hole transport solution in an amount which accounts for 1% of the total solution mass, adding 4-tert-butylpyridine in an amount which accounts for 2% of the total solution mass, adding chlorobenzene in an amount which accounts for 65% of the total solution mass, adding Spiro-OMeTAD (hole transport material) in an amount which accounts for 32% of the total solution mass, and dropwise adding the Spiro-OMeTAD solution into PEO and ZnO modified organic-inorganic hybrid perovskite CH 3 NH 3 SnClI 2 Obtaining a hole transport layer on the surface of the light absorption layer in a spin coating mode, wherein the spin coating process is set to 3500 rpm for 25 s;
(5) And evaporating a thin metal counter electrode on the surface of the hole transport layer: and (3) performing vacuum evaporation on the silver counter electrode with the thickness of 60 nm at the speed of 0.4 nm/s by adopting a vacuum evaporation method to obtain the silver counter electrode.
The performance of the translucent flexible organic-inorganic hybrid perovskite solar cell based on polymer and inorganic oxide nanoparticles obtained in this example was tested: in a room temperature environment, the humidity is more than 60 percent, a xenon lamp is used for simulating sunlight, and the light intensity is 100 mW/cm 2 The effective illumination area is 0.25 cm 2 The photoelectric conversion efficiency of the photoelectric conversion element is 21%, after the element is placed for 300 days under the condition of no packaging, the photoelectric efficiency is reduced to 96% of the initial value, and 92% of the initial efficiency can still be maintained after 3500 times of circular bending (the bending radius is 3 mm).
Example 3
This example uses Polymer (PMMA) and inorganic nano-oxide nanoparticles (Al) 2 O 3 ) The embodiment is based on a method for improving flexibility and mechanical property of a flexible perovskite solar cell, and when the conductive substrate is defined as the lowest layer, the method sequentially comprises the following steps from bottom to top: a transparent ITO-PEN conductive substrate; a zinc dioxide electron transport layer; with PMMA (polymer) and Al 2 O 3 (inorganic oxide nanoparticles) modified inorganic perovskite CsPbI 3 A light absorbing layer; a hole transport layer; a gold counter electrode.
The embodiment is based on a method for improving the flexibility and mechanical properties of a semitransparent flexible perovskite solar cell, and the preparation method comprises the following steps:
(1) Cleaning transparent ITO-PEN to obtain a transparent conductive substrate: respectively adopting deionized water, absolute ethyl alcohol and isopropanol to ultrasonically vibrate for 15 min to clean the ITO-PEN conductive substrate, placing the ITO-PEN conductive substrate into an oven to be dried for 15 min at 100 ℃ after ultrasonic treatment to remove visible impurities on the surface, and then treating the ITO-PEN conductive substrate on an ultraviolet ozone treatment machine for 20 min to remove organic groups on the surface so as to reduce a water contact angle;
(2) Preparing a zinc dioxide electron transport layer on the surface of the transparent conductive substrate obtained in the step (1): dropwise adding zinc dioxide dispersion liquid on the transparent conductive substrate after ozone treatment, carrying out spin coating at 5000 rpm for 25 s by using a spin coating method to uniformly form a film, heating on a heating table at 180 ℃ for 35 min to obtain a zinc dioxide electronic transmission layer, wherein the zinc dioxide colloid dispersion liquid is prepared by mixing zinc dioxide colloid and deionized water according to a volume ratio of 1:2, mixing and ultrasonically dispersing;
(3) Preparing PMMA and Al on the surface of the zinc dioxide electron transport layer obtained in the step (2) 2 O 3 Modified inorganic perovskite CsPbI 3 A light absorbing layer;
(3-I) mixing PMMA and Al 2 O 3 And the molar ratio is 1:1 CsI and PbI 2 Dissolving in dimethyl sulfoxide (DMSO) solution, heating at 70 deg.C and stirring for 8 hr to obtain PEO and ZnO modified inorganic perovskite precursor solution, wherein the addition amount of PMMA is 10% of total mass, and Al is 2 O 3 The amount of CsI added corresponds to 10% of the total mass, the amount of CsI added corresponds to 20% of the total mass, and PbI 2 The addition amount of (2) is equivalent to 20% of the total mass, and the addition amount of the DMSO solvent is equivalent to 40% of the total mass;
(3-II) mixing PMMA obtained in the step (3-I) and Al 2 O 3 Filtering the modified inorganic perovskite precursor solution by a filter head with the diameter of 0.45 mu m, then dripping the modified inorganic perovskite precursor solution on the zinc dioxide electron transport layer obtained in the step (2), and obtaining PMMA and Al in a spin coating mode 2 O 3 Modified inorganic materialsPerovskite CsPbI 3 The light absorption layer is set to 4500 rpm,30s by a spin coating process; adding 300 mu L of chlorobenzene solution when the solution is poured for 25 s by spin coating, carrying out heat treatment for 10 min at 160 ℃, and annealing to obtain a smooth perovskite film;
(4) PMMA and Al obtained in step (3) 2 O 3 Modified inorganic perovskite CsPbI 3 Preparing a hole transport layer on the surface of the light absorbing layer: adding lithium bis (trifluoromethanesulfonylimide) in the hole transport solution in an amount which accounts for 1.5% of the total solution mass, adding 4-tert-butylpyridine in an amount which accounts for 2.8% of the total solution mass, adding chlorobenzene in an amount which accounts for 64% of the total solution mass, adding Spiro-OMeTAD (hole transport material) in an amount which accounts for 31.7% of the total solution mass, and dropwise adding the Spiro-OMeTAD solution into PEO and ZnO modified inorganic perovskite CsPbI 3 Obtaining a hole transport layer on the surface of the light absorption layer in a spin coating mode, wherein the spin coating process is set to 3500 rpm for 30s;
(5) And evaporating a thin metal counter electrode on the surface of the hole transport layer: vacuum evaporating at 0.3 nm/s speed to form 60 nm silver counter electrode.
The performance of the resulting polymer and inorganic oxide nanoparticle-based translucent flexible inorganic perovskite solar cell of this example was tested: in a room temperature environment, the humidity is less than 30 percent, a xenon lamp is used for simulating sunlight, and the light intensity is 100 mW/cm 2 The effective illumination area is 0.25 cm 2 The photoelectric conversion efficiency of the packaging material is 16%, after the packaging material is placed for 150 days under the non-packaging condition, the photoelectric efficiency is reduced to 90% of the initial value, and 94% of the initial efficiency can be still maintained after the packaging material is circularly bent for 3000 times (the bending radius is 3 mm).
Comparative example 1 (comparison with example 1)
The comparative example, which is based on a method for improving the flexibility and mechanical properties of a flexible perovskite solar cell, defined as the lowest layer of a conductive substrate, includes, in order from bottom to top: a transparent ITO-PEN conductive substrate; a tin dioxide electron transport layer; organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 A light absorbing layer; a hole transport layer; a gold counter electrode.
The comparative example is based on a method for improving the flexibility and mechanical properties of a semitransparent flexible perovskite solar cell, and the preparation method comprises the following steps:
(1) Cleaning transparent ITO-PEN to obtain a transparent conductive substrate: respectively adopting deionized water, absolute ethyl alcohol and isopropanol to ultrasonically vibrate for 10 min to clean the ITO-PEN conductive substrate, placing the ITO-PEN conductive substrate into an oven to be dried for 15 min at 100 ℃ after ultrasonic treatment to remove visible impurities on the surface, and then treating the ITO-PEN conductive substrate on an ultraviolet ozone treatment machine for 25 min to remove organic groups on the surface so as to reduce a water contact angle;
(2) Preparing a tin dioxide electron transport layer on the surface of the transparent conductive substrate obtained in the step (1): dropwise adding tin dioxide colloid dispersion liquid on the transparent conductive substrate after ozone treatment, uniformly forming a film by spin coating at 5000 rpm for 20 s, and heating at 160 ℃ for 35 min on a heating table to obtain a tin dioxide electronic transmission layer, wherein the tin dioxide colloid dispersion liquid is prepared by mixing tin dioxide colloid and deionized water according to a volume ratio of 1:4, mixing and ultrasonically dispersing;
(3) Preparing organic-inorganic hybrid perovskite CH on the surface of the stannic oxide electron transport layer obtained in the step (2) 3 NH 3 PbI 3 A light absorbing layer;
(3-I) mixing the components in a molar ratio of 1:1 CH 3 NH 3 I and PbI 2 Dissolved in a solvent with the volume ratio of 1:4, heating and stirring at 60 ℃ for 12 h to obtain an organic-inorganic hybrid perovskite precursor solution, wherein CH is contained in the precursor solution 3 NH 3 The addition of I is 18% of the total mass, pbI 2 The amount of the DMSO solvent is equal to 57% of the total mass;
(3-II) filtering the organic-inorganic perovskite precursor liquid obtained in the step (3-I) through a filter head with the diameter of 0.22 mu m, then dropwise adding the organic-inorganic perovskite precursor liquid on the tin dioxide electron transport layer obtained in the step (2), and obtaining the organic-inorganic hybrid perovskite CH in a spin coating mode 3 NH 3 PbI 3 A light absorption layer, wherein the spin coating process is set to be 5000 rpm for 30s; adding 250 μ L ethyl acetate solution when the amount is 23 s, heat treating at 110 deg.C for 10 min, and removingObtaining a smooth perovskite film by fire;
(4) The organic-inorganic hybrid perovskite CH obtained in the step (3) 3 NH 3 PbI 3 Preparing a hole transport layer on the surface of the light absorbing layer: adding lithium bis (trifluoromethanesulfonylimide) in the hole transport solution in an amount which accounts for 1.5% of the total solution mass, adding 4-tert-butylpyridine in an amount which accounts for 2.5% of the total solution mass, adding chlorobenzene in an amount which accounts for 66% of the total solution mass, adding Spiro-OMeTAD (hole transport material) in an amount which accounts for 30% of the total solution mass, and dropwise adding the Spiro-OMeTAD solution to organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 Obtaining a hole transport layer on the surface of the light absorption layer in a spin coating mode, wherein the spin coating process is set to 3000 rpm for 30s;
(5) And evaporating a thin metal counter electrode on the surface of the hole transport layer: and (3) performing vacuum evaporation on the silver counter electrode with the thickness of 40 nm at the speed of 0.3 nm/s by adopting a vacuum evaporation method, and thus obtaining the silver electrode.
The performance of the semitransparent flexible inorganic perovskite solar cell obtained by the comparative example was tested: in a room temperature environment, the humidity is more than 50 percent, a xenon lamp is used for simulating sunlight, and the light intensity is 100 mW/cm 2 The effective illumination area is 0.25 cm 2 The photoelectric conversion efficiency of the packaging material is 14%, after the packaging material is placed for 30 days under the non-packaging condition, the photoelectric efficiency is reduced to 12% of the initial value, and 10% of the initial efficiency can be still maintained after the packaging material is circularly bent for 500 times (the bending radius is 3 mm).
COMPARATIVE EXAMPLE 2 (in contrast to EXAMPLE 1)
The comparative example, which is based on a method for improving the flexibility and mechanical properties of a flexible perovskite solar cell, defined as the lowest layer of a conductive substrate, includes, in order from bottom to top: a transparent ITO-PEN conductive substrate; a tin dioxide electron transport layer; organic-inorganic hybrid perovskite CH modified by chitosan 3 NH 3 PbI 3 A light absorbing layer; a hole transport layer; a gold counter electrode.
The comparative example is based on a method for improving the flexibility and mechanical properties of a semitransparent flexible perovskite solar cell, and the preparation method comprises the following steps:
(1) Cleaning transparent ITO-PEN to obtain a transparent conductive substrate: respectively adopting deionized water, absolute ethyl alcohol and isopropanol to ultrasonically vibrate for 10 min to clean the ITO-PEN conductive substrate, putting the ITO-PEN conductive substrate into an oven to be dried for 15 min at 100 ℃ after ultrasonic treatment to remove visible impurities on the surface, and then treating the ITO-PEN conductive substrate on an ultraviolet ozone processor for 25 min to remove organic groups on the surface so as to reduce a water contact angle;
(2) Preparing a tin dioxide electron transport layer on the surface of the transparent conductive substrate obtained in the step (1): dropwise adding tin dioxide colloid dispersion liquid on the transparent conductive substrate after ozone treatment, uniformly forming a film by spin coating at 5000 rpm for 20 s, and heating at 160 ℃ for 35 min on a heating table to obtain a tin dioxide electronic transmission layer, wherein the tin dioxide colloid dispersion liquid is prepared by mixing tin dioxide colloid and deionized water according to a volume ratio of 1:4, mixing and ultrasonically dispersing;
(3) Preparing organic-inorganic hybrid perovskite CH on the surface of the stannic oxide electron transport layer obtained in the step (2) 3 NH 3 PbI 3 A light absorbing layer;
(3-I) mixing chitosan in a molar ratio of 1:1 CH 3 NH 3 I and PbI 2 Dissolving in a solvent with the volume ratio of 1:4, heating and stirring at 60 ℃ for 12 h to obtain an organic-inorganic hybrid perovskite precursor solution, wherein the addition of the chitosan is 1% of the total mass, and CH is added 3 NH 3 The addition of I is 18 percent of the total mass, pbI 2 The amount of the DMSO solvent is 25% of the total mass, and the amount of the DMSO solvent is 56% of the total mass;
(3-II) filtering the organic-inorganic perovskite precursor liquid obtained in the step (3-I) through a filter head with the diameter of 0.22 mu m, then dropwise adding the organic-inorganic hybrid perovskite precursor liquid on the tin dioxide electron transmission layer obtained in the step (2), and obtaining the organic-inorganic hybrid perovskite CH in a spin coating mode 3 NH 3 PbI 3 A light absorption layer, wherein the spin coating process is set to be 5000 rpm for 30s; adding 250 mu L of ethyl acetate solution when the solution is poured for 23 s by spin coating, carrying out heat treatment at 110 ℃ for 10 min, and annealing to obtain a smooth perovskite film;
(4) The organic-inorganic hybrid perovskite CH obtained in the step (3) 3 NH 3 PbI 3 Preparing a hole transport layer on the surface of the light absorbing layer: adding lithium bis (trifluoromethanesulfonylimide) in the hole transport solution in an amount which accounts for 1.5% of the total solution mass, adding 4-tert-butylpyridine in an amount which accounts for 2.5% of the total solution mass, adding chlorobenzene in an amount which accounts for 66% of the total solution mass, adding Spiro-OMeTAD (hole transport material) in an amount which accounts for 30% of the total solution mass, and dropwise adding the Spiro-OMeTAD solution to organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 Obtaining a hole transport layer on the surface of the light absorption layer in a spin coating mode, wherein the spin coating process is set to 3000 rpm for 30s;
(5) And evaporating a thin metal counter electrode on the surface of the hole transport layer: and (3) performing vacuum evaporation on the silver counter electrode with the thickness of 40 nm at the speed of 0.3 nm/s by adopting a vacuum evaporation method, and thus obtaining the silver electrode.
The polymer-based translucent flexible inorganic perovskite solar cell obtained in this comparative example was tested for performance: in a room temperature environment, the humidity is more than 60 percent, a xenon lamp is used for simulating sunlight, and the light intensity is 100 mW/cm 2 The effective illumination area is 0.25 cm 2 The photoelectric conversion efficiency of the LED is 16%, after the LED is placed for 200 days under the non-packaging condition, the photoelectric efficiency is reduced to 32% of the initial value, and 20% of the initial efficiency can be still maintained after 1500 times of circular bending (the bending radius is 3 mm).
COMPARATIVE EXAMPLE 3 (in contrast to EXAMPLE 1)
This comparative example uses inorganic oxide nanoparticles to modify a perovskite layer, and when a conductive substrate is defined as the lowermost layer based on a method for improving the flexibility and mechanical properties of a flexible perovskite solar cell, includes, in order from bottom to top: a transparent ITO-PEN conductive substrate; a tin dioxide electron transport layer; with TiO as a carrier 2 (inorganic oxide nanoparticles) modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 A light absorbing layer; a hole transport layer; a gold counter electrode.
The comparative example is based on a method for improving the flexibility and mechanical properties of a flexible perovskite solar cell, and the preparation method comprises the following steps:
(1) Cleaning transparent ITO-PEN to obtain a transparent conductive substrate: respectively adopting deionized water, absolute ethyl alcohol and isopropanol to ultrasonically vibrate for 10 min to clean the ITO-PEN conductive substrate, putting the ITO-PEN conductive substrate into an oven to be dried for 15 min at 100 ℃ after ultrasonic treatment to remove visible impurities on the surface, and then treating the ITO-PEN conductive substrate on an ultraviolet ozone processor for 25 min to remove organic groups on the surface so as to reduce a water contact angle;
(2) Preparing a tin dioxide electron transport layer on the surface of the transparent conductive substrate obtained in the step (1): dropwise adding tin dioxide colloid dispersion liquid on the transparent conductive substrate after ozone treatment, carrying out spin coating for 20 s at 5000 rpm by using a spin coating method to uniformly form a film, heating for 35 min at 160 ℃ on a heating table to obtain a tin dioxide electronic transmission layer, wherein the tin dioxide colloid dispersion liquid is prepared from tin dioxide colloid and deionized water according to a volume ratio of 1:4, mixing and ultrasonically dispersing;
(3) Preparing TiO on the surface of the stannic oxide electron transport layer obtained in the step (2) 2 Modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 A light absorbing layer;
(3-I) adding TiO 2 The molar ratio is 1:1 CH 3 NH 3 I and PbI 2 Dissolving in a solvent with the volume ratio of 1:4 in a mixed solution of dimethyl sulfoxide (DMSO) and N, N-Dimethylformamide (DMF), heating and stirring at 60 ℃ for 12 hours to obtain TiO 2 Modified organic-inorganic hybrid perovskite precursor solution, in which TiO is 2 Is added in an amount of 3% of the total mass, CH 3 NH 3 The addition of I is equal to 15 percent of the total mass, and PbI 2 The addition amount of (2) is 22% of the total mass, the addition amount of the DMSO solvent is 13% of the total mass, and the addition amount of the DMF solvent is 50% of the total mass;
(3-II) subjecting the TiO obtained in the step (3-I) 2 Filtering the modified organic-inorganic hybrid perovskite precursor solution by a filter head with the diameter of 0.22 mu m, then dropwise adding the filtered solution on the stannic oxide electron transport layer obtained in the step (2), and obtaining TiO by a spin coating mode 2 Modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 A light absorption layer, wherein the spin coating process is set to be 5000 rpm for 30s; adding 250 mu L of ethyl acetate solution when the solution is poured for 23 s by spin coating, carrying out heat treatment at 100 ℃ for 10 min, and annealing to obtain a smooth perovskite film;
(4) In thatTiO obtained in the step (3) 2 Modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 Preparing a hole transport layer on the surface of the light absorbing layer: adding lithium bis (trifluoromethanesulfonylimide) in the hole transport solution in an amount which accounts for 1.5% of the total solution mass, adding 4-tert-butylpyridine in an amount which accounts for 2.5% of the total solution mass, adding chlorobenzene in an amount which accounts for 66% of the total solution mass, adding P3HT (hole transport material) in an amount which accounts for 30% of the total solution mass, and dropwise adding the P3HT solution to TiO 2 Modified organic-inorganic hybrid perovskite CH 3 NH 3 PbI 3 Obtaining a hole transport layer on the surface of the light absorption layer in a spin coating mode, setting a spin coating process at 3000 rpm for 30s;
(5) And evaporating a thin metal counter electrode on the surface of the hole transport layer: vacuum evaporating at 0.4 nm/s rate for 40 nm gold counter electrode.
The performance of the semitransparent flexible organic-inorganic hybrid perovskite solar cell based on inorganic oxide nanoparticles obtained in the comparative example was tested: in a room temperature environment, the humidity is more than 50 percent, a xenon lamp is used for simulating sunlight, and the light intensity is 100 mW/cm 2 The effective illumination area is 0.25 cm 2 The photoelectric conversion efficiency of the packaging material is 15%, after the packaging material is placed for 100 days under the non-packaging condition, the photoelectric efficiency is reduced to 30% of the initial value, and 45% of the initial efficiency can be still maintained after the packaging material is circularly bent for 2000 times (the bending radius is 3 mm).
Claims (10)
1. A method for improving the flexibility and mechanical property of a flexible perovskite solar cell is characterized in that when a conductive substrate is defined as the lowest layer, the solar cell sequentially comprises the following components from bottom to top: a conductive substrate layer; an electron transport layer; a polymer and inorganic metal oxide nanoparticle modified perovskite light-absorbing layer; a hole transport layer; and a counter electrode.
2. The method of improving the flexibility and mechanical properties of a flexible perovskite solar cell as claimed in claim 1, wherein the conductive substrate layer is a transparent polyethylene naphthalate flexible substrate; the electron transport layer is SnO 2 、TiO 2 ZnO or PA CBM electron transport layer; the hole transport layer is one or more of Spiro-OMeTAD, PSS, P3HT, PEDOT and NiO; the polymer is one or more of chitosan, polyethylene oxide, polyacrylonitrile, polymethyl methacrylate and poly (vinylidene fluoride-co-hexafluoropropylene); the inorganic metal nano oxide is TiO 2 、ZnO、Al 2 O 3 、SiO 2 And ZrO 2 One or more of the above; the perovskite light absorption layer is ABX 3 Perovskite light-absorbing layer, wherein A is CH 3 NH 3 Or Cs, B is Pb, sn, in or Ge, and X is one or more of I, br or Cl.
3. The method for improving the flexibility and mechanical properties of a flexible perovskite solar cell according to claim 1 or 2, characterized in that the method comprises the following steps:
(1) Cleaning a transparent polyethylene terephthalate flexible substrate to prepare a transparent conductive substrate;
(2) Preparing an electron transport layer on the surface of the prepared conductive substrate;
(3) Preparing polymer and inorganic metal oxide nanoparticle modified perovskite ABX on surface of prepared electron transport layer 3 A light absorbing layer;
(4) Perovskite ABX modified on prepared polymer and inorganic metal oxide nanoparticles 3 Preparing a hole transport layer on the surface of the light absorption layer;
(5) And (3) evaporating a thin metal counter electrode on the surface of the prepared hole transport layer.
4. The method for improving the flexibility and mechanical properties of the flexible perovskite solar cell according to claim 3, wherein in the step (1), the cleaning manner is as follows: and (3) placing the transparent FTO conductive glass in deionized water, absolute ethyl alcohol and isopropanol, respectively performing ultrasonic oscillation for 10-20 min, baking for 10-25 min at 80-120 ℃, and performing ultraviolet ozone treatment for 20-30 min.
5. Improved flexible perovskites according to claim 3 or 4The method for improving the flexibility and the mechanical property of the solar cell is characterized in that in the step (2), the preparation method of the electron transport layer comprises the following steps: dripping the electronic transmission material dispersion liquid on the surface of the conductive substrate, spin-coating at 4000-6000 rpm for 20-40 s, and heating at 150-200 ℃ for 30-40 min to obtain the conductive substrate; the electron transport material dispersion is made of an electron transport material (SnO) 2 、TiO 2 ZnO or PCBM) and a solvent (deionized water or isopropanol or chlorobenzene) in a volume ratio of 1: mixing 1 to 8, and performing ultrasonic dispersion to prepare the material.
6. The method for improving the flexibility and the mechanical property of the flexible perovskite solar cell according to any one of claims 3 to 5, wherein in the step (3), the perovskite precursor solution after being filtered is dripped on the surface of the electron transmission layer, and the perovskite light absorption layer is obtained through spin coating, heat treatment and annealing; the preparation method of the perovskite precursor liquid comprises the following steps: mixing polymer, inorganic oxide nanoparticles, AX and BX 2 Dissolving the mixture in dimethyl sulfoxide or a solution of N, N-dimethylformamide, and heating and stirring at 65 to 75 ℃ for 4 to 12 hours.
7. The method for improving the flexibility and the mechanical property of the flexible perovskite solar cell as claimed in claim 6, wherein in the step (3), the addition amount of the polymer in the perovskite precursor liquid is 0 to 10 percent of the total mass of the precursor liquid, the addition amount of the inorganic metal oxide nanoparticles is 0 to 10 percent of the total mass of the precursor liquid, the addition amount of AX is 10 to 20 percent of the total mass of the precursor liquid, and BX is 10 to 20 percent of the total mass of the precursor liquid 2 The addition amount of the N, N-dimethylformamide is 20% -50% of the total mass of the precursor liquid; the diameter of a filter head used for filtering is 0.22 to 0.45
(ii) a The rotation speed of the spin coating is 3500 to 7500 rpm, and the time is 20 to 40 s; adding 200-300 parts of the mixture into the solution after the solution is spun until the countdown is 10-24 s
Methyl acetate, ethyl acetate or chlorobenzene solution; the temperature of the heat treatment is 70 to 200 ℃, and the time is 5 to 20 min.
8. The method for improving the flexibility and the mechanical property of the flexible perovskite solar cell according to any one of claims 3 to 7, wherein in the step (4), the hole transport solution is dripped on the surface of the perovskite light absorption layer, and spin coating is performed to obtain the hole transport layer.
9. The method for improving the flexibility and the mechanical property of the flexible perovskite solar cell as claimed in claim 8, wherein in the step (4), in the hole transport solution, the mass of lithium bistrifluoromethanesulfonylimide is 0.2 to 2% of the total mass of the solution, the mass of 4-tert-butylpyridine is 0.8 to 3% of the total mass of the solution, the mass of chlorobenzene is 60 to 80% of the total mass of the solution, and the mass of the hole transport material is 10 to 30% of the total mass of the solution; the rotation speed of the spin coating is 2000 to 3500 rpm, and the time is 30 to 40 s.
10. The method for improving the flexibility and the mechanical property of the flexible perovskite solar cell according to any one of claims 3 to 9, characterized in that in the step (5), a thin metal counter electrode is evaporated by a vacuum evaporation method; the vacuum evaporation rate is 0.1 to 0.6 nm/s, and the thickness of the thin metal counter electrode is 10 to 60 nm; the counter electrode is gold or silver.
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