CN111584715A - Modifier, perovskite active material, preparation method and perovskite solar cell - Google Patents

Modifier, perovskite active material, preparation method and perovskite solar cell Download PDF

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Publication number
CN111584715A
CN111584715A CN202010255899.7A CN202010255899A CN111584715A CN 111584715 A CN111584715 A CN 111584715A CN 202010255899 A CN202010255899 A CN 202010255899A CN 111584715 A CN111584715 A CN 111584715A
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perovskite
modifier
polymethyl methacrylate
ionic liquid
fullerene derivative
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CN202010255899.7A
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Inventor
向昱任
屈军乐
宋军
彭晓
于德良
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Shenzhen University
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Shenzhen University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/20—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising organic-organic junctions, e.g. donor-acceptor junctions
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
    • H10K85/211—Fullerenes, e.g. C60
    • H10K85/215—Fullerenes, e.g. C60 comprising substituents, e.g. PCBM
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Photovoltaic Devices (AREA)

Abstract

The invention discloses a modifier, a perovskite active material, a preparation method and a perovskite solar cell. The modifier comprises a fullerene derivative, polymethyl methacrylate and organic ionic liquid, and the halide perovskite is modified by the combination of the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid, so that the photoelectric response characteristic and the environmental stability of the halide perovskite are improved, and the performance of the perovskite solar cell is finally improved. The preparation method comprises the steps of contacting halide perovskite with a multi-element organic molecular modifier, and carrying out annealing treatment to prepare the perovskite thin film material with excellent photoelectric properties. The method has the advantages of simple process and high repeatability, and can optimize the multielement organic molecular components according to the actual application requirements so as to exert the photoelectric property of the halide perovskite thin film to the maximum extent and realize excellent device performance.

Description

Modifier, perovskite active material, preparation method and perovskite solar cell
Technical Field
The invention belongs to the technical field of perovskite material preparation, and particularly relates to a modifier, a perovskite active material, a preparation method and a perovskite solar cell.
Background
Since the first report of perovskite solar cells, the cell efficiency of the perovskite solar cells is rapidly improved from the initial 3.8% to 25%. The improvement of efficiency benefits from the improvement of the perovskite thin film preparation process, wherein the Anti-solvent method (Anti-solvent method) greatly improves the quality of the thin film and provides guarantee for preparing a high-efficiency battery. Meanwhile, researches find that the chemical properties of the film grain boundary and the defects thereof have important influence on the generation, collection and transportation of carriers. In addition, the perovskite thin film is susceptible to external light, heat, water and oxygen to cause the performance of the material to be reduced and even degraded, thereby seriously affecting the performance of the device and the commercial application thereof.
How to further improve the photoelectric property and the environmental stability of the perovskite thin film through an interface modification technology has become a technical key point in the current field.
Disclosure of Invention
Therefore, the invention provides a multi-element organic molecule modifier, a perovskite active material and a preparation method thereof, and aims to solve the technical problem that the photoelectric property and the environmental stability of the perovskite thin film are improved through interface modification.
Therefore, the invention provides the following technical scheme:
the multi-element organic molecule modifier provided by the invention comprises a fullerene derivative, polymethyl methacrylate and organic ionic liquid.
Further, the mass ratio of the fullerene derivative to the polymethyl methacrylate to the organic ionic liquid is (0.1-3): (0.1-1): (1-8).
Further, the fullerene derivative is [6,6 ]]-phenyl-C61-methyl butyrate and/or [6,6 ]]-phenyl-C71-methyl butyrate;
the organic ionic liquid is trioctylammonium trifluoromethanesulfonate and/or methyl imidazole chloride.
Further, the weight average molecular weight of the polymethyl methacrylate is 80000-120000.
Further, the composite material also comprises an organic solvent, wherein the concentration of the fullerene derivative in a mixture formed by the organic solvent, the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid is 0.1-3mg/ml, the concentration of the polymethyl methacrylate is 0.1-1mg/ml, and the concentration of the organic ionic liquid is 1-8 mg/ml.
In addition, the invention also provides a perovskite active material which comprises the multielement organic molecule modifier.
In addition, the invention also provides a preparation method of the perovskite active material, which comprises the following steps: the halide perovskite is contacted with a multi-element organic molecule modifier, and annealing treatment is carried out to prepare the perovskite active material.
Further, the contacting may occur between the halide perovskite precursor solution, the in-process perovskite thin film, the formed perovskite thin film, and the polyhydric organic molecule modifier, and may be accomplished in one or more steps.
Further, the temperature of the annealing treatment is 70-150 ℃, and the time is 30-120 min; preferably, the temperature of the annealing treatment is 90-110 ℃, and the time is 55-65 min;
the annealing treatment is carried out in at least one atmosphere of nitrogen, oxygen, carbon dioxide, dimethyl sulfoxide and dimethylformamide.
Further, the halide perovskite has the chemical formula ABX3Wherein A is a cation; b is at least one of lead and tin atoms; x is a halogen ion.
In addition, the invention also provides a perovskite solar cell which comprises the perovskite active material or the perovskite active material prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) the modifier provided by the invention comprises a fullerene derivative, polymethyl methacrylate and organic ionic liquid, and the halide perovskite is modified by matching the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid, so that the influence degree of external factors on the performance of the perovskite thin film can be reduced, the photoelectric response performance is improved, and the performance of the perovskite solar cell is finally improved.
(2) The modifier provided by the invention utilizes the fullerene derivative to provide an electron extraction function, utilizes the polymethyl methacrylate to provide a water vapor barrier effect, and utilizes the organic ionic liquid to provide ion compensation and defect passivation effects. By limiting the proportion of the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid, the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid are compatible, and the performances of all components are fully exerted: the excessive fullerene derivative will cause the reduction of the parallel resistance and the increase of the leakage current of the device, while the excessive polymethyl methacrylate will increase the series resistance, and the excessive organic ionic liquid will cause the reduction of the stability and the filling factor of the device.
(3) The preparation method of the perovskite active material provided by the invention comprises the steps of contacting halide perovskite with a multi-element organic molecular modifier, and carrying out annealing treatment to prepare the perovskite active material; specifically, the mass ratio of the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid is reasonably configured, and the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid are mixed with a halide perovskite precursor liquid or added into a perovskite active material (namely a halide perovskite active layer) through an anti-solvent to prepare the perovskite thin film material with excellent photoelectric properties. The method has the advantages of simple process and high repeatability, and can optimize the multielement organic molecular components according to the actual application requirements so as to exert the photoelectric property of the halide perovskite thin film to the maximum extent and realize excellent device performance.
(4) According to the preparation method of the perovskite active material, the photoelectric response performance of the perovskite thin film is improved through crystal boundary modification, and the morphology and the photoelectric performance of the perovskite thin film can be reasonably regulated and controlled.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic structural view of a perovskite solar cell in example 1 of the present invention;
FIG. 2 is a graph of the efficiency of a perovskite solar cell of the present invention;
FIG. 3 is an X-ray diffraction pattern of a perovskite thin film modified with a modifier in example 1 of the present invention and a perovskite thin film unmodified with a modifier in comparative example 1;
FIG. 4 is a scanning electron micrograph of a perovskite thin film modified with a modifier in example 1 of the present invention;
FIG. 5 is a scanning electron micrograph of a perovskite thin film which is not modified by a modifier in comparative example 1 of the present invention.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be purchased in the market.
The perovskite in each of the following examples and comparative examples has the chemical formula ABX3Wherein A is a cation; b is at least one of lead and tin atoms; x is a halogen ion.
The weight average molecular weight of polymethyl methacrylate is 80000-120000.
Example 1
The embodiment provides a perovskite solar cell and a preparation method thereof. The preparation method comprises the following steps:
(1) lead iodide (PbI) is added in an anhydrous environment (environment with a relative humidity of less than 30 wt.%) to the reaction mixture2) Dissolving iodomethylamine (MAI) in a mixed solvent of Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) to prepare a perovskite precursor solution with the molar concentration of 2M; wherein the molar ratio of the lead iodide to the iodomethylamine is 1: 1.10; the volume ratio of the dimethyl formamide to the dimethyl sulfoxide is 4: 1;
(2) under the anhydrous environment (or the environment with the relative humidity less than 30wt percent), the fullerene derivative- [6,6 ]]-phenyl-C61Methyl butyrate, polymethyl methacrylate and trioctyl ammonium triflate are sequentially added into chlorobenzene for full dissolution, and then a 0.45-micron filter head is adopted for filtration, so as to prepare the modifier containing the multielement organic molecules; wherein, the concentration of the fullerene derivative is 1.8mg/ml, the concentration of the polymethyl methacrylate is 0.6mg/ml, and the concentration of the trioctyl ammonium trifluoromethanesulfonate is 4.5 mg/ml;
(3) under the anhydrous environment (or the environment with the relative humidity less than 30 wt%), the perovskite precursor solution is coated on a pretreated substrate (PEDOT: PSS/ITO glass) in a spinning mode at the rotating speed of 6000rpm, after 20-25s of spinning (the total spinning time is 30s), an anti-solvent (chlorobenzene) is quickly dripped, and after the spinning is finished, the substrate is quickly placed on a 100 ℃ hot bench for annealing for 20min to prepare the perovskite thin film;
(4) spin-coating a modifier containing multiple organic molecules on the surface of the perovskite thin film prepared in the step (2) for 30s at the rotating speed of 3000rpm to obtain the perovskite thin film with the surface covered with the modifier;
(5) placing the perovskite thin film with the surface covered with the modifier in a DMSO atmosphere, and annealing for 60min at 100 ℃ to facilitate growth of perovskite grains and permeation modification of organic molecules to the grain boundary of the thin film to prepare the perovskite thin film modified by the modifier, namely a perovskite active layer consisting of perovskite active materials;
(6) under an anhydrous environment (or an environment with relative humidity less than 30 wt%), a chlorobenzene solution of PCBM and an ethanol solution of BCP are sequentially coated on the perovskite active layer in a spin coating mode, so that an electron transport layer and a buffer layer are sequentially formed; wherein the concentration of PCBM in chlorobenzene solution of PCBM is 25mg/ml, the rotating speed of spin coating is 2000rpm, and the time is 30 s; the concentration of BCP in the ethanol solution of BCP is 5mg/ml, the rotation speed of spin coating is 6000rpm, and the time is 30 s;
and then silver is evaporated on the surface of the buffer layer to form a silver electrode with the thickness of 100nm, so that the perovskite solar cell with the inverted structure is manufactured, the structural schematic diagram of the perovskite solar cell is shown in figure 1, and part of the structure is not shown in figure 1.
Example 2
The embodiment provides a perovskite solar cell and a preparation method thereof. The preparation method is the same as that of example 1, except that: in the step (2), the fullerene derivative is [6,6 ]]-phenyl-C71-methyl butyrate, the fullerene derivative at a concentration of 1.0mg/ml, polymethyl methacrylate at a concentration of 0.5mg/ml, trioctylammonium trifluoromethanesulfonate at a concentration of 1.5 mg/ml; in the step (4), the spin coating rotating speed is 2000 rpm; and (5) the atmosphere is DMF atmosphere, the annealing temperature is 110 ℃, and the time is 40 min.
Example 3
The embodiment provides a perovskite solar cell and a preparation method thereof. The preparation method is the same as that of example 1, except that: in the step (3), the modifier containing the multielement organic molecules, which is prepared in the step (2), is adopted to replace the antisolvent (chlorobenzene); the steps after omitting step (4) were the same as in example 1.
Example 4
The embodiment provides a perovskite solar cell and a preparation method thereof. The preparation method is the same as that of the example 1, and the only difference is that: in example 4, 0.1mg/ml of polymethyl methacrylate was previously dissolved in the perovskite precursor solution in step (1) of example 1, and no polymethyl methacrylate was added to the polybasic organic modifier in step (2) of example 1.
Example 5
The embodiment provides a perovskite solar cell and a preparation method thereof. The preparation method is different from that of the example 1 in that in the step (3), under the anhydrous environment (or the environment with the relative humidity less than 30 wt%), the ethanol solution (0.5mg/ml) of the polymethyl methacrylate is preferentially coated on the pretreated substrate (PTAA/ITO glass) in a rotating speed of 6000rpm, and the interface barrier layer is formed after heat treatment at 100 ℃ for 5 min. And spin-coating the perovskite precursor solution on the polymethyl methacrylate barrier layer at the rotating speed of 6000rpm, quickly dropwise adding an anti-solvent (chlorobenzene) after spin-coating for 20-25s (the total spin-coating time is 30s), and quickly placing the substrate on a 100 ℃ hot bench for annealing for 20min after the spin-coating is finished to obtain the perovskite thin film. The remaining steps were the same as in example 1.
Comparative example 1
The present comparative example provides a perovskite solar cell and a method of fabricating the same. The only difference from example 1 is that: the perovskite thin film in this comparative example was not modified with a modifier containing multiple organic molecules.
Test examples
The perovskite solar cells prepared in example 1, example 4 and comparative example 1 were tested for their respective properties, and the test results were as follows:
wherein, fig. 2 is a graph of efficiency of the perovskite solar cell of the present invention, and it can be known from fig. 2 that: the perovskite thin film processed by the organic modifier can obviously improve the conversion efficiency of the perovskite solar cell.
Wherein, fig. 3 is an X-ray diffraction pattern of the perovskite thin film modified by the modifier in the embodiment 1 of the invention and the perovskite thin film without the modifier in the comparative example 1, and it can be known from fig. 3 that: the multielement organic modifier does not obviously change the crystal form of the perovskite thin film.
FIG. 4 is a scanning electron microscope image of the perovskite thin film modified by the modifier in example 1 of the present invention; FIG. 5 is a scanning electron micrograph of a perovskite thin film which is not modified by a modifier in comparative example 1 of the present invention. As can be seen from fig. 4 and 5: after the perovskite thin film is modified by adopting a multi-element organic modifier, the crystal grains of the perovskite thin film are obviously increased.
From the above test results, it can be known that: the perovskite thin film prepared by the modifier has more excellent photoelectric characteristics and environmental stability, and the efficiency of the perovskite battery is improved.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims (10)

1. A modifier comprises a fullerene derivative, polymethyl methacrylate and organic ionic liquid.
2. The modifying agent according to claim 1, wherein the mass ratio of the fullerene derivative, the polymethyl methacrylate, and the organic ionic liquid is (0.1-3): (0.1-1): (1-8).
3. The modifying agent according to claim 1 or 2, wherein said fullerene derivative is [6,6]-phenyl-C61-methyl butyrate and/or [6,6 ]]-phenyl-C71-methyl butyrate;
the organic ionic liquid is trioctylammonium trifluoromethanesulfonate and/or methyl imidazole chloride.
4. The modifying agent as claimed in any one of claims 1 to 3, wherein the weight average molecular weight of the polymethyl methacrylate is 80000-120000.
5. The modifier according to any one of claims 2 to 4, further comprising an organic solvent, wherein the concentration of the fullerene derivative in the mixture of the organic solvent, the fullerene derivative, the polymethyl methacrylate and the organic ionic liquid is 0.1 to 3mg/ml, the concentration of the polymethyl methacrylate is 0.1 to 1mg/ml, and the concentration of the organic ionic liquid is 1 to 8 mg/ml.
6. A perovskite active material comprising the modifier according to any one of claims 1 to 4.
7. A method of preparing the perovskite active material as claimed in claim 6, comprising the steps of:
the halide perovskite is contacted with a modifier, and annealing treatment is carried out to prepare the perovskite material modified by the multielement organic molecules.
8. The method according to claim 7, wherein the annealing treatment is carried out at a temperature of 70 to 150 ℃ for 30 to 120 min;
the annealing treatment is carried out in at least one atmosphere of nitrogen, oxygen, carbon dioxide, dimethyl sulfoxide and dimethylformamide.
9. The production method according to claim 7 or 8, wherein the halide perovskite has a chemical formula of ABX3Wherein A is a cation; b is at least one of lead and tin atoms; x is a halogen ion.
10. A perovskite solar cell comprising the perovskite active material according to claim 6 or the perovskite active material produced by the production method according to any one of claims 7 to 9.
CN202010255899.7A 2020-04-02 2020-04-02 Modifier, perovskite active material, preparation method and perovskite solar cell Pending CN111584715A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113611802A (en) * 2021-08-30 2021-11-05 南京工业大学 Perovskite solar cell modified by organic small molecules, preparation method and application

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CN110729403A (en) * 2019-11-13 2020-01-24 山西大学 Preparation method and application of high-quality organic-inorganic hybrid perovskite film
CN110854272A (en) * 2019-11-21 2020-02-28 重庆大学 Ternary halogen perovskite solar cell and preparation method thereof

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CN110729403A (en) * 2019-11-13 2020-01-24 山西大学 Preparation method and application of high-quality organic-inorganic hybrid perovskite film
CN110854272A (en) * 2019-11-21 2020-02-28 重庆大学 Ternary halogen perovskite solar cell and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113611802A (en) * 2021-08-30 2021-11-05 南京工业大学 Perovskite solar cell modified by organic small molecules, preparation method and application
CN113611802B (en) * 2021-08-30 2023-10-31 南京工业大学 Perovskite solar cell modified by small organic molecules, preparation method and application

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Application publication date: 20200825