CN112467041A - Interface modification method of perovskite/carbon electrode - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 46
- 238000002715 modification method Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000004528 spin coating Methods 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000010409 thin film Substances 0.000 claims description 21
- 239000010408 film Substances 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 8
- -1 amine halogen compound Chemical class 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012296 anti-solvent Substances 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 150000002366 halogen compounds Chemical class 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229910003472 fullerene Inorganic materials 0.000 claims description 2
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000002161 passivation Methods 0.000 claims description 2
- 229940071182 stannate Drugs 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 229910052718 tin Inorganic materials 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 229910052791 calcium Inorganic materials 0.000 claims 1
- 239000011575 calcium Substances 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- OWPISBZHEXGKAZ-UHFFFAOYSA-N C1(=CC=CC=C1)CCN.[I] Chemical class C1(=CC=CC=C1)CCN.[I] OWPISBZHEXGKAZ-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052731 fluorine Inorganic materials 0.000 abstract description 2
- 239000011737 fluorine Substances 0.000 abstract description 2
- 125000001153 fluoro group Chemical group F* 0.000 abstract description 2
- 229910003471 inorganic composite material Inorganic materials 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000007547 defect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/88—Passivation; Containers; Encapsulations
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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
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/81—Electrodes
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- 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
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Abstract
An interface modification method of perovskite/carbon electrode belongs to the technical field of organic-inorganic composite materials and photoelectric materials. The main steps are that after the perovskite film is prepared by one-step spin coating method, fluorine substituted phenylethylamine iodine (F-PEAI) is adopted to grow in situ (F-PEA) on the perovskite film2PbI4The perovskite surface is improved in a two-dimensional layer mode, the perovskite/carbon electrode interface can be improved based on the coated carbon electrode, and the assembled carbon-based perovskite solar cell has high photoelectric conversion efficiency. The material preparation method provided by the invention has the advantages of low cost, good stability, simple preparation process, strong controllability and repeatability, and is suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of organic-inorganic composite materials and photoelectric materials, and particularly relates to an interface modification method of a perovskite/carbon electrode and application of the interface modification method in carbon-based perovskite solar cells (C-PSCs).
Background
In recent years, the problem of energy shortage is increasingly highlighted, and the traditional fossil energy is limited in storage and non-renewable, and can bring huge pollution to the environment in the using process. This also promotes the development and utilization of renewable energy resources, and solar energy is receiving more and more attention as a clean and renewable energy source. Under the background, great interest of researchers in various countries is caused by the development of novel high-efficiency low-cost solar cells, and particularly, perovskite solar cells are developed rapidly from 3.8% of efficiency, which is developed in 2009, to 25.5% of efficiency, which is developed rapidly, by virtue of good light absorption and fast charge transfer rate, and great development potential, and are known as "new hopes in the photovoltaic field". The film with the thickness of hundreds of nanometers in the perovskite solar cell can fully absorb sunlight with the wavelength of below 800nm, and the density and the flatness of the film greatly influence the separation and the transmission of photon-generated carriers in the perovskite solar cell. In addition, in order to solve the stability problems of organic hole transport layers (HTMs) and metal electrodes in conventional PSCs and improve the stability of PSCs, several electrodes with hole extraction capability have been developed to prepare PSCs devices without HTMs, including Au, Ni, and Carbon (Carbon). Among them, carbon materials are considered as the most promising electrode materials because they are inexpensive, stable in properties, inert to ion migration, and inherently water-repellent, which all contribute to the improvement in the stability of PSCs. However, the perovskite/carbon electrode interface in the C-PSCs device has poor contact and a large number of gap defects exist at the perovskite/carbon electrode interface, which can hinder hole extraction, resulting in charge recombination. Therefore, it is necessary to provide an interface modification method for improving the interface contact between perovskite/carbon electrodes, which is beneficial to improving the efficiency and stability of carbon-based perovskite solar cells.
Disclosure of Invention
The invention aims to provide an interface modification method of a perovskite/carbon electrode and application of the interface modification method in a carbon-based perovskite solar cell. In situ growth (F-PEA) on perovskite thin films by spin coating fluorine substituted phenethylamine iodine (F-PEAI) solutions2PbI4The two-dimensional layer is coated on the basis of the carbon electrode, so that the interface contact between perovskite/carbon electrodes is improved, and the assembled carbon-based perovskite solar cell has good photoelectric conversion efficiency and good stability.
The invention provides an interface modification method of a perovskite/carbon electrode, which comprises the following specific steps:
1) preparation of perovskite precursor solution:
RMX3the preparation method of the perovskite precursor solution comprises the steps of preparing an organic amine halogen compound RX and a metal halogen compound MX2Mixing the mixture into an organic solvent, and stirring the mixture overnight at normal temperature to obtain a clear and transparent yellow solution.
2) Preparing a three-dimensional perovskite thin film:
in a glove box, RMX is put in3Preparing a perovskite precursor adduct film on a conductive substrate or a conductive substrate coated with a current carrier transmission thin layer by a one-step spin-coating film forming method and a method of dropwise adding an anti-solvent, annealing and cooling to room temperature;
3) two-dimensional (F-PEA)2PbI4Preparation of the layer:
preparation (F-PEA)2PbI4Followed by growing the passivation layer in situ (F-PEA)2PbI4Spin-coating the solution on the three-dimensional perovskite film obtained in the step 2), and drying the film in the air to improve the quality of the perovskite film;
4) then in two dimensions (F-PEA)2PbI4The carbon electrode is coated on the layer for annealing, so that the aim of improving the interface contact between the perovskite/carbon electrode is fulfilled.
Applications in solar cells: the 2D/3D mixed perovskite thin film is applied to a carbon-based perovskite solar cell structure.
Step 1): the R group in RX is selected from CH3NH3、NH2-CH＝NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3、HC(NH2)2、C6H5(CH2)2NH3One of the groups; x in RX is one of I, Br and Cl. Wherein the organic amine halogen compound is selected from one, two or a mixture of more of the RX compounds.
MX2The metal M in the alloy is one of Pb and Sn; the anion X in the metal salt compound is I, Br,One of Cl; the metal halogen compound is selected from MX2One, two or a mixture of several of the above.
The RX and MX2In a molar ratio of 1:1, RX and MX2The mass percentage of the perovskite precursor solution is preferably 35-40 wt%.
The organic solvent is a mixed solvent of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), and the volume fraction of the DMSO in the organic solvent is 5-15 vol%.
The antisolvent in the step 2) is chlorobenzene, toluene, diethyl ether, cyclohexane or a mixed solvent of the chlorobenzene, the toluene, the diethyl ether and the cyclohexane. The dripping method is dripping at constant speed 6s before the spin coating is finished to form a strand of continuous liquid.
The conductive substrate is FTO conductive glass, ITO conductive glass or a flexible conductive substrate.
The electron transport layer is made of zinc oxide, tin dioxide, titanium dioxide, lanthanum-doped barium stannate, fullerene and derivatives.
Annealing treatment on the heating plate is heating for 5-10 min at 25-120 ℃.
The concentration of the isopropanol solution of the F-PEAI in the step 3) is 0.5-8 mg/mL, and the concentration is 2.25cm2The three-dimensional perovskite film corresponds to an isopropanol solution of 40-100 mu L F-PEAI, and the spin coating speed of the isopropanol solution of F-PEAI is 2000-6000 r.p.m.
And 4) uniformly coating a layer of carbon slurry on the prepared film, and annealing at 80-100 ℃ for 10-60 min to assemble the carbon-based perovskite solar cell.
Compared with the prior art, the invention has the following beneficial effects:
1) the DMSO-based organic lead halogen perovskite precursor solution has the advantages of low cost, simple operation and high repeatability;
2) according to the DMSO-based organolead halide perovskite thin film, a 2D perovskite thin film is grown in situ on the perovskite thin film through spin coating of a fluorine-substituted PEAI solution (F-PEAI) to play a role in passivating a grain boundary and reducing the defect state density of the thin film, meanwhile, the energy band of the perovskite thin film can be regulated and controlled, the interface contact between perovskite/carbon electrodes is improved, and fewer relevant reports are provided for perovskite/carbon electrode interface modification through the strategy. Experiments show that the carbon-based perovskite solar cell assembled by the method has higher photoelectric conversion efficiency.
Drawings
FIG. 1, SEM of a carbon-based perovskite thin film material prepared in example 1 without F-PEAI treatment.
FIG. 2 is a scanning electron micrograph of the F-PEAI-based treated carbon-based perovskite thin film material prepared in example 1.
FIG. 3 is an I-V curve of a solar cell made of the carbon-based perovskite thin film material prepared in example 1.
Detailed Description
The invention is further illustrated by the following figures and examples, but is not limited to the following examples.
Example 1
1) Preparation of perovskite precursor solution:
will CH3NH3I:PbI2The DMSO molar ratio is 1:1:1, and the DMSO is dissolved in the DMF solution, and the specific formula is as follows: 461mg of PbI2、159mg CH3NH3I and 78mg DMSO (70.9. mu.L) were dissolved in 600mg DMF (632.9. mu.L) solvent, placed in a nitrogen glove box environment, and stirred overnight at room temperature to give a perovskite precursor solution.
2) Preparing a perovskite thin film:
in a glove box, the perovskite precursor solution obtained in step 1) was spin-coated on an ETL substrate at 4000rpm for 20s, and 0.5mL of diethyl ether was continuously and slowly dropped onto the rotating substrate during the spin-coating process to accelerate the volatilization of the solvent DMF. Then, the perovskite thin film is annealed at 95 ℃ for 5 min. Then spin-coating 70 μ L (area of perovskite thin film is 2.25 cm) on the perovskite thin film at a rotation speed of 5000r.p.m2) And F-PEAI isopropanol solution with the concentration of 4mg/mL, and performing surface modification on the perovskite film to finally obtain the 2D/3D mixed perovskite film.
3) Applications in solar cells:
and uniformly coating a layer of carbon slurry on the prepared perovskite film, and then annealing for 30min at 100 ℃ to prepare the carbon-based perovskite solar cell.
As can be seen from fig. 1 and 2, based on the 2D/3D perovskite thin film material grown in situ by F-PEAI, a 2D perovskite layer is formed on the surface of the thin film to cover the grain boundary of the bottom perovskite, so that the defects at the grain boundary are passivated, and the formed two-dimensional layer increases the roughness of the surface of the perovskite thin film, increases the contact area between the carbon electrode and the perovskite thin film, and thus improves the perovskite/carbon electrode interface contact.
As can be seen from FIG. 3, the carbon-based perovskite solar cell assembled based on 2D/3D perovskite thin film material is under standard light source (AM 1.5G,100 mW/cm)2) The current-voltage curve of the cell is measured, and the photoelectric conversion efficiency is higher, and is improved from the initial 11.5% to 13.4%.
Claims (9)
1. The interface modification method of the perovskite/carbon electrode is characterized by comprising the following specific steps:
1) preparation of perovskite precursor solution:
RMX3the preparation method of the perovskite precursor solution comprises the steps of preparing an organic amine halogen compound RX and a metal halogen compound MX2Mixing the mixture into an organic solvent, and stirring the mixture overnight at normal temperature to obtain a clear and transparent yellow solution;
2) preparing a three-dimensional perovskite thin film:
in a glove box, RMX is put in3Preparing a perovskite precursor adduct film on a conductive substrate or a conductive substrate coated with a current carrier transmission thin layer by a one-step spin-coating film forming method and a method of dropwise adding an anti-solvent, annealing and cooling to room temperature;
3) two-dimensional (F-PEA)2PbI4Preparation of the layer:
preparation (F-PEA)2PbI4Followed by growing the passivation layer in situ (F-PEA)2PbI4Spin-coating the solution on the three-dimensional perovskite film obtained in the step 2), and drying the film to improve the calcium and titanium contentThe quality of the ore film;
4) then in two dimensions (F-PEA)2PbI4The carbon electrode is coated on the layer for annealing, so that the aim of improving the interface contact between the perovskite/carbon electrode is fulfilled.
2. The method for modifying the interface of a perovskite/carbon electrode as claimed in claim 1, wherein the step 1): the R group in RX is selected from CH3NH3、NH2-CH＝NH2、CH3CH2NH3、CH3(CH2)2NH3、CH3(CH2)3NH3、HC(NH2)2、C6H5(CH2)2NH3One of the groups; x in RX is one of I, Br and Cl, wherein the organic amine halogen compound is selected from one, two or a mixture of the RX; MX2The metal M in the alloy is one of Pb and Sn; the anion X in the metal salt compound is one of I, Br and Cl; the metal halogen compound is selected from MX2One, two or a mixture of several of the above.
3. The method for interfacial modification of a perovskite/carbon electrode as claimed in claim 1, wherein the RX, MX in step 1) are2In a molar ratio of 1:1, RX and MX2The mass percentage of the perovskite precursor solution is preferably 35-40 wt%.
4. The interface modification method for perovskite/carbon electrode according to claim 1, wherein the organic solvent in step 1) is a mixed solvent of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), and volume fraction of DMSO in the organic solvent is 5-15 vol%.
5. The interface modification method of a perovskite/carbon electrode according to claim 1, wherein the anti-solvent in step 2) is chlorobenzene, toluene, diethyl ether, cyclohexane or a mixed solvent thereof; the dripping method is dripping the mixture in uniform speed 6s before the spin coating is finished to form a strand of continuous liquid;
the conductive substrate is FTO conductive glass, ITO conductive glass or a flexible conductive substrate;
the electron transport layer is made of zinc oxide, tin dioxide, titanium dioxide, lanthanum-doped barium stannate, fullerene and derivatives.
6. The interface modification method of a perovskite/carbon electrode as claimed in claim 1, wherein the annealing treatment in step 2) on the heating plate is heating at 25-120 ℃ for 5-10 min.
7. The interface modification method of a perovskite/carbon electrode as claimed in claim 1, wherein the concentration of the isopropanol solution of the F-PEAI in the step 3) is 0.5 to 8mg/mL per 2.25cm2The three-dimensional perovskite film corresponds to an isopropanol solution of 40-100 mu L F-PEAI, and the spin coating speed of the isopropanol solution of F-PEAI is 2000-6000 r.p.m.
8. The interface modification method of the perovskite/carbon electrode as claimed in claim 1, wherein step 4) is to uniformly blade coat a layer of carbon slurry on the prepared film, anneal for 10-60 min at 80-100 ℃, and assemble the carbon-based perovskite solar cell.
9. A perovskite/carbon electrode obtainable by a process as claimed in any one of claims 1 to 8.
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| CN114805150A (en) * | 2022-05-09 | 2022-07-29 | 山西大学 | Interface modification molecule applied to lead-based perovskite solar cell |
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| CN111540808A (en) * | 2020-04-03 | 2020-08-14 | 华南师范大学 | Method for preparing high-efficiency carbon electrode inorganic perovskite solar cell by using phenylalkylamine derivative |
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| Publication number | Priority date | Publication date | Assignee | Title |
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