CN110649161A - Method for preparing high-purity and high-flatness perovskite film by using mixed solvent - Google Patents

Method for preparing high-purity and high-flatness perovskite film by using mixed solvent Download PDF

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Publication number
CN110649161A
CN110649161A CN201910868589.XA CN201910868589A CN110649161A CN 110649161 A CN110649161 A CN 110649161A CN 201910868589 A CN201910868589 A CN 201910868589A CN 110649161 A CN110649161 A CN 110649161A
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pbi
purity
solution
flatness
thin film
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陈海宁
刘慧丛
李卫平
朱立群
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Beihang University
Beijing University of Aeronautics and Astronautics
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Beijing University of Aeronautics and Astronautics
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/42Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for sensing infra-red radiation, light, electro-magnetic radiation of shorter wavelength or corpuscular radiation and adapted for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation using organic materials as the active part, or using a combination of organic materials with other material as the active part; Multistep processes for their manufacture
    • H01L51/4213Comprising organic semiconductor-inorganic semiconductor hetero-junctions
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/0001Processes specially adapted for the manufacture or treatment of devices or of parts thereof
    • H01L51/0002Deposition of organic semiconductor materials on a substrate
    • H01L51/0003Deposition of organic semiconductor materials on a substrate using liquid deposition, e.g. spin coating
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention provides a method for preparing a high-purity and high-flatness perovskite thin film by using a mixed solvent. The preparation method of the perovskite thin film comprises the following steps: mixing isopropanol and isooctane to obtain a mixed solvent A; will CH3NH3Dissolving I in a solvent A to obtain a solution B for conversion; will PbI2Dissolving in DMF to obtain a precursor solution C; spin-coating the solution C on a solar cell substrate, and annealing to obtain PbI2A precursor film; will PbI2Putting the precursor film in the solution B for conversion, and annealing to obtain CH3NH3PbI3A perovskite thin film. The invention is realized by adding in CH3NH3I, introducing isooctane solvent into isopropanol solution to promote PbI2Precursor to CH3NH3PbI3The perovskite is converted, and the purity and the flatness of the perovskite film are improved.

Description

Method for preparing high-purity and high-flatness perovskite film by using mixed solvent
Technical Field
The invention relates to CH3NH3PbI3A process for the preparation of perovskites, in particular CH by chemical conversion in perovskites3NH3I Isooctane is added into isopropanol solution to prepare high-purity and high-flatness CH3NH3PbI3A perovskite thin film.
Background
Perovskite solar cells based on solution fabrication techniques have received much attention because of their high conversion efficiency. The quality of the perovskite thin film prepared by the solution method seriously influences the conversion efficiency of the solar cell. The two-step process is an important method for preparing perovskite thin films, namely PbI is firstly deposited on a battery substrate2Precursor film, and placing the precursor film in CH3NH3Chemical conversion of the solution I to obtain CH3NH3PbI3A perovskite thin film.
At present, CH in the second step of the process3NH3The solvent used for the solution I is generally isopropanol, and the medium polarity solvent hardly makes PbI difficult to be dissolved in the conversion process2Complete conversion of precursor into CH3NH3PbI3Perovskite, and cause a dissolution recrystallization process during the conversion process, so that the thin film becomes rough. For this purpose, CH with high purity and high flatness is prepared3NH3PbI3Perovskite thin films are a problem that needs to be solved at present.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing high purity and high flatness perovskite thin film by using mixed solvent, and particularly relates to a method for preparing high purity and high flatness perovskite thin film by using mixed solvent in CH3NH3I, introducing isooctane solvent into isopropanol solution to promote PbI2Precursor to CH3NH3PbI3The perovskite is converted, the purity of the perovskite thin film is improved, and meanwhile, the flatness of the thin film is improved.
In order to achieve the above purpose, the invention provides the following technical scheme:
the method for preparing the perovskite thin film with high purity and high flatness by using the mixed solvent comprises the following steps:
(1) mixing isopropanol and isooctane to obtain a mixed solvent A;
(2) will CH3NH3Dissolving I in the solvent A obtained in the step (1) to obtain a solution B for conversion;
(3) will PbI2Dissolving in DMF to obtain a precursor solution C;
(4) spin-coating the solution C obtained in the step (3) on a solar cell substrate, and annealing to obtain PbI2A precursor film;
(5) the PbI obtained in the step (4) is treated2Putting the precursor film in the solution B for conversion, and annealing to obtain CH3NH3PbI3A perovskite thin film.
Further, the volume ratio of isopropanol to isooctane in the solvent A is 1: 0.1-20.
Further, the volume ratio of isopropanol to isooctane in the solvent A is 1: 9.
further, CH in solution B3NH3The dosage range of I is 0.001-20 mg/mL.
Further, CH in solution B3NH3I is 0.1 mg/mL.
Further, PbI in solution C2The dosage range is 0.3-1.5 mol/L.
Further, in the step (4), the spin coating speed is 1000rpm/min to 4000rpm/min.
Further, in the step (4), the spin coating time is 10-30 s.
Further, in the step (4), the annealing temperature is 70-150 ℃ and the time is 2-15 min.
Further, in the step (5), the conversion reaction time is 10min-12h, the annealing temperature is 80-120 ℃, and the time is 3-20 min.
Compared with the prior art, the invention has the beneficial effects that:
(1) PbI used in the present invention2、CH3NH3I. Materials such as isopropanol, isooctane and DMF are all common industrial raw materials; the whole process is simple and convenient, easy to operate and suitable for large-scale production;
(2) the mixed solvent of isopropanol and isooctane adopted in the invention has the advantages of good solubilityExhibiting low solvent polarity in PbI2To CH3NH3PbI3During perovskite conversion, previously converted CH may be suppressed3NH3PbI3The dissolution and recrystallization processes avoid the generation of large-size crystal grains, effectively reduce the roughness of the film and obtain a more compact film with high flatness;
(3) the mixed solvent of isopropanol and isooctane adopted in the invention effectively inhibits CH in the conversion process3NH3PbI3To PbI2And CH3NH3The reverse transformation process of I increases PbI2To CH3NH3PbI3The driving force of the conversion is to obtain high-purity CH3NH3PbI3A film;
(4) the mixed solvent of isopropanol and isooctane adopted in the invention leads PbI to be2To CH3NH3PbI3The conversion process can be at a lower CH3NH3I concentration, thereby reducing CH in the whole conversion process3NH3Waste of material I.
Drawings
FIG. 1 is an XRD pattern of a sample obtained in example 1.
Fig. 2 is an XRD pattern of the sample obtained in example 2.
Fig. 3 is an XRD pattern of the sample obtained in comparative example 1.
Fig. 4 is an XRD pattern of the sample obtained in comparative example 2.
FIG. 5 is a scanning electron microscope photograph of a sample obtained in example 1.
FIG. 6 is a scanning electron microscope photograph of a sample obtained in comparative example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of protection of the present invention.
Example 1
The method for preparing the perovskite thin film with high purity and high flatness by using the mixed solvent specifically comprises the following steps:
(1) mixing isopropanol and isooctane according to a volume ratio of 1: 9 mixing to obtain a solvent A;
(2) adding 0.1mg/mL of CH3NH3Dissolving I in the solvent A obtained in the step (1) to obtain a solution B for conversion;
(3) 1.2mol/L of PbI2Dissolving in DMF to obtain a precursor solution C;
(4) spin-coating the solution C obtained in the step (3) on a solar cell substrate at the spin-coating speed of 2000rpm/min, and annealing at 100 ℃ for 5min to obtain PbI2A precursor film;
(5) the PbI obtained in the step (4) is treated2The precursor film is placed in the solution B for conversion, the conversion time is 2h, and the CH is obtained by annealing treatment for 10min at 100 DEG C3NH3PbI3A perovskite thin film.
The XRD pattern of the sample obtained in example 1 is shown in FIG. 1, and the sample obtained in example 1 has a perovskite structure, good crystallinity and no appearance of PbI2The purity of the sample is higher; the scanning electron micrograph of the sample obtained in example 1 is shown in fig. 5, and it can be seen that the surface topography of the sample is high in flatness, and the sample covers the entire plane.
Example 2
The method for preparing the perovskite thin film with high purity and high flatness by using the mixed solvent specifically comprises the following steps:
(1) mixing isopropanol and isooctane according to a volume ratio of 1: 5 mixing to obtain a solvent A;
(2) adding 0.1mg/mL of CH3NH3Dissolving I in the solvent A obtained in the step (1) to obtain a solution B for conversion;
(3) 1.2mol/L of PbI2Dissolving in DMF to obtain a precursor solution C;
(4) spin-coating the solution C obtained in the step (3) on a solar cell substrate at a spin-coating speedThe temperature is 2000rpm/min, and the PbI is obtained by annealing treatment at 100 ℃ for 5min2A precursor film;
(5) the PbI obtained in the step (4) is treated2The precursor film is placed in the solution B for conversion, the conversion time is 2h, and the CH is obtained by annealing treatment for 10min at 100 DEG C3NH3PbI3A perovskite thin film.
The XRD pattern of the sample obtained in example 2 is shown in FIG. 2, the sample obtained in example 2 is of perovskite structure, the diffraction peak of perovskite is still strong, namely perovskite with higher purity is still obtained, but PbI with low strength can be observed2Diffraction peaks, indicating the presence of a small amount of PbI2
Comparative example 1
The method for preparing the perovskite thin film specifically comprises the following steps:
(1) isopropanol is used as a solvent A;
(2) adding 0.1mg/mL of CH3NH3Dissolving I in the solvent A obtained in the step (1) to obtain a solution B for conversion;
(3) 1.2mol/L of PbI2Dissolving in DMF to obtain a precursor solution C;
(4) spin-coating the solution C obtained in the step (3) on a solar cell substrate at the spin-coating speed of 2000rpm/min, and annealing at 100 ℃ for 5min to obtain PbI2A precursor film;
(5) the PbI obtained in the step (4) is treated2The precursor film is placed in the solution B for conversion, the conversion time is 2h, and the CH is obtained by annealing treatment for 10min at 100 DEG C3NH3PbI3A perovskite thin film.
The XRD pattern of the sample obtained in comparative example 1 is shown in fig. 3, and the sample obtained in comparative example 1 has no characteristic diffraction peak of perovskite, and only strong PbI is observed2Diffraction peaks, indicating that no conversion occurred.
Comparative example 2
The method for preparing the perovskite thin film specifically comprises the following steps:
(1) isopropanol is used as a solvent A;
(2) will be 10mg/mL CH3NH3Dissolving I in the solvent A obtained in the step (1) to obtain a solution B for conversion;
(3) 1.2mol/L of PbI2Dissolving in DMF to obtain a precursor solution C;
(4) spin-coating the solution C obtained in the step (3) on a solar cell substrate at the spin-coating speed of 2000rpm/min, and annealing at 100 ℃ for 5min to obtain PbI2A precursor film;
(5) the PbI obtained in the step (4) is treated2The precursor film is placed in the solution B for conversion, the conversion time is 2h, and the CH is obtained by annealing treatment for 10min at 100 DEG C3NH3PbI3A perovskite thin film.
The XRD pattern of the sample obtained in comparative example 2 is shown in FIG. 4, the sample obtained in comparative example 2 is of a perovskite structure, the perovskite characteristic diffraction peak has stronger intensity and better crystallinity, but PbI can still be observed2Diffraction peaks, indicating that the sample purity is still not high; the scanning electron micrograph of the sample obtained in comparative example 2 is shown in fig. 6, and it can be seen that the surface of the sample is very rough, and many large-sized perovskite crystals appear.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.

Claims (10)

1. The method for preparing the perovskite thin film with high purity and high flatness by using the mixed solvent is characterized by comprising the following steps:
(1) mixing isopropanol and isooctane to obtain a mixed solvent A;
(2) will CH3NH3Dissolving I in the solvent A obtained in the step (1) to obtain a solution B for conversion;
(3) will PbI2Dissolving in DMF to obtain a precursor solution C;
(4) spin-coating the solution C obtained in the step (3) on a solar cell substrate, and annealing to obtain PbI2A precursor film;
(5) the PbI obtained in the step (4) is treated2Putting the precursor film in the solution B for conversion, and annealing to obtain CH3NH3PbI3A perovskite thin film.
2. The method for preparing a high-purity and high-flatness perovskite thin film by using the mixed solvent as claimed in claim 1, wherein the volume ratio of isopropanol to isooctane in the solvent A is 1: 0.1-20.
3. The method for preparing a high-purity and high-flatness perovskite thin film by using the mixed solvent as claimed in claim 2, wherein the volume ratio of isopropanol to isooctane in the solvent A is 1: 9.
4. the method for preparing high-purity and high-flatness perovskite thin film by using mixed solvent as claimed in claim 1, wherein CH in solution B3NH3The dosage range of I is 0.001-20 mg/mL.
5. The method for preparing high-purity and high-flatness perovskite thin film by using mixed solvent as claimed in claim 4, wherein CH in solution B3NH3I is 0.1 mg/mL.
6. The method for preparing a high-purity and high-flatness perovskite thin film by using the mixed solvent as claimed in claim 1, wherein PbI is contained in the solution C2The dosage range is 0.3-1.5 mol/L.
7. The method for preparing a high-purity and high-flatness perovskite thin film by using the mixed solvent as claimed in claim 1, wherein in the step (4), the spin coating speed is 1000rpm/min to 4000rpm/min.
8. The method for preparing a high-purity and high-flatness perovskite thin film by using the mixed solvent as claimed in claim 1, wherein in the step (4), the spin coating time is 10-30 s.
9. The method for preparing a high-purity and high-flatness perovskite thin film by using the mixed solvent as claimed in claim 1, wherein in the step (4), the annealing temperature is 70-150 ℃ and the annealing time is 2-15 min.
10. The method for preparing a high-purity and high-flatness perovskite thin film by using the mixed solvent as claimed in claim 1, wherein in the step (5), the conversion reaction time is 10min-12h, the annealing temperature is 80-120 ℃, and the annealing time is 3-20 min.
CN201910868589.XA 2019-09-16 2019-09-16 Method for preparing high-purity and high-flatness perovskite film by using mixed solvent Pending CN110649161A (en)

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