CN108682745A - A method of perovskite thin film is prepared based on anti-solvent dynamic spin coating - Google Patents
A method of perovskite thin film is prepared based on anti-solvent dynamic spin coating Download PDFInfo
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- H—ELECTRICITY
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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
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
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Abstract
In a kind of method preparing perovskite thin film based on anti-solvent dynamic spin coating proposed by the present invention, a kind of organic solvent of dissolvable lead iodide is chosen, a kind of insoluble perovskite material but dissolve each other with lead iodide solvent and can dissolve CH3NH3The solvent of I (MAI) is as anti-solvent (such as isopropanol)；The aqueous isopropanol of MAI is added dropwise during the DMF solution of spin coating lead iodide, by controlling the dripping quantity of the aqueous isopropanol of MAI and opportunity being added dropwise, the crystalline condition of perovskite thin film can be controlled, finally obtain the perovskite thin film of high quality.The perovskite thin film surfacing obtained in coarse mesoporous Grown using the method for the present invention is fine and close, and pin-free, crystallite dimension greatly reduces loss of the carrier in grain boundaries up to a few micrometers, is conducive to application of the perovskite material in photoelectric field.
Description
Technical field
The present invention relates to the preparation methods of perovskite thin film, and in particular to one kind preparing calcium titanium based on anti-solvent dynamic spin coating
The method of mine film.
Background technology
Hybrid inorganic-organic perovskite material (CH3NH3PBX3, X=Cl, Br, I) and it is used as a kind of emerging photovoltaic semiconductors material
Material has the excellent photoelectric properties such as direct band gap, the high absorption coefficient of light, high carrier mobility and free path.From 2009,
It is such new after Organic-inorganic composite halide perovskite material is applied to photoelectric field by Japanese Scientists Miyasaka for the first time
Type photoelectric material gradually enters into the visual field of researcher and on the peak for welcoming concern in recent years.It is based particularly on the calcium of such material
Titanium ore based solar battery, its transfer efficiency is flushed to 23% again within 2018, alreadys exceed current commercialized monocrystalline silicon
Based solar battery.Meanwhile perovskite-based solar cell prepares work relative to traditional silicon substrate, GaAs based solar battery
Skill is simpler, lower cost for material, is known as solar cell with the fastest developing speed so far.
The crystallization of perovskite light absorbing layer and quality of forming film have the performance of perovskite-based solar cell vital
It influences, it is therefore, particularly important to the exploration of perovskite thin film preparation process.Currently, the preparation method of perovskite material is mainly：
It steams the vapor phase method for representative altogether with double source, reacts to be spin-coated as the liquid phase method represented and mixed-powder and to form consolidating for perovskite
Xiang Fa.Wherein, vapor phase method is not appropriate for industrializing extensive life due to needing the limiting factors such as vacuum, high temperature evaporation high energy consumption
Production.And solid phase method is often confined to powder preparation, is not suitable for forming a film.Liquid phase method be based particularly on the liquid phase method of spin coating proceeding due to
Its advantage such as of low cost, simple for process, easily controllable, becomes and studies widest method at present.Spin-coating method includes mainly one
Walk solwution method and step deposition, wherein a step solwution method is to prepare the common method of perovskite, i.e., by PbI2And CH3NH3I
(MAI) it is scattered according to a certain percentage in n,N-Dimethylformamide and is configured to orange-yellow precursor liquid, existed using the method for spin coating
Film forming is prepared on substrate, removing excess of solvent by annealing makes perovskite crystalline.But the method crystallization process is difficult to control, and is obtained
The perovskite thin film crystalline quality arrived is poor.Although being proposed in follow-up study calcium titanium is assisted using anti-solvents such as chlorobenzene, ether
Mine forms a film, but the crystalline quality of the perovskite thin film to being formed on the larger mesoporous substrate of roughness does not improve.In order to
Improve the crystalline quality of the perovskite thin film formed on the larger mesoporous substrate of roughness, Gratzel seminars propose substep
Sedimentation, i.e., by PbI2And CH3NH3Two kinds of predecessors of I are sequentially deposited on substrate so that the two is reacted on substrate
Form perovskite thin film.This method can effectively control the crystallization process of perovskite, and so that perovskite film layer and mesoporous substrate have good
Good compatibility, but the perovskite thin film crystal grain prepared is fine crushing.
Invention content
It is an object of the present invention to brilliant for the existing perovskite thin film in coarse mesoporous Grown of background technology
Grain problem fine crushing, it is proposed that a method of perovskite thin film is prepared based on anti-solvent dynamic spin coating.Using this method thick
The perovskite thin film surfacing that rough mesoporous Grown obtains is fine and close, and pin-free, crystallite dimension drops significantly up to a few micrometers
Low loss of the carrier in grain boundaries, is conducive to application of the perovskite material in photoelectric field.
In a kind of method preparing perovskite thin film based on anti-solvent dynamic spin coating proposed by the present invention, choose a kind of solvable
It solves the organic solvent (such as DMF) of lead iodide, a kind of insoluble perovskite material but dissolves each other and can dissolve with lead iodide solvent
CH3NH3The solvent of I (MAI) is as anti-solvent (such as isopropanol)；It is added dropwise MAI's during the DMF solution of spin coating lead iodide
Aqueous isopropanol can control the crystallization of perovskite thin film by controlling the dripping quantity of the aqueous isopropanol of MAI and opportunity being added dropwise
Situation finally obtains the perovskite thin film that large area is smooth, pin-free, crystal grain reaches micron level.
The technical solution adopted by the present invention is as follows：
A method of perovskite thin film is prepared based on anti-solvent dynamic spin coating, specifically includes following steps：
Step 1, cleaning substrate；
Step 2 by solute, organic solvent of lead iodide is solvent, prepares the iodate that mass concentration is 0.3~0.6g/mL
Lead solution；With iodine methylamine (CH3NH3I, MAI) it is used as solute, isopropanol as solvent, preparation mass concentration is 30~70mg/mL
Iodine methylamine aqueous isopropanol；
Step 3, the iodate lead solution for preparing step 2 10~15min of the pre-heat treatment at 60~70 DEG C；
Step 4 forms perovskite thin film using spin-coating method on the substrate after step 1 is cleaned, and spin coating rotating speed is
3000rpm, time 30s；Detailed process is：First, on the substrate that step 1 cleans up after 3 the pre-heat treatment of a dropping step
Iodate lead solution, start spin coating；The aqueous isopropanol for the iodine methylamine that a dropping step 2 is prepared after 5~25s of spin coating continues spin coating,
Wherein, the volume ratio of iodate lead solution and the aqueous isopropanol of iodine methylamine is (0.6~1.6)：1；During continuing spin coating, iodine
The aqueous isopropanol of methylamine is reacted with lead iodide generates perovskite, and toasted processing, removes residual solution and surface layer excess MAI is obtained
To perovskite thin film.
Further, substrate described in step 1 is the electro-conductive glass of having electronic transport layer.
Further, the process of cleaning substrate described in step 1 is specially：A. successively by the electro-conductive glass of having electronic transport layer
It is cleaned by ultrasonic in acetone, alcohol, water, dries；B. to the electro-conductive glass of upper step treated having electronic transport layer carry out it is ultraviolet-
Ozone treatment, to increase the hydrophily of substrate.
Further, organic solvent described in step 2 be DMF (n,N-Dimethylformamide), DMSO (dimethyl sulfoxide (DMSO)), or
The mixed solvent of person DMF and DMSO.
Further, step 2 to step 4 is carried out in the glove box of nitrogen atmosphere.
Further, when step 4 uses spin-coating method to form perovskite thin film on the substrate after step 1 cleaning, acceleration
For 1000rpm/s.
Compared with prior art, beneficial effects of the present invention are：
1, the present invention provides a kind of methods preparing perovskite thin film based on anti-solvent dynamic spin coating, first, prepare iodine
Change the aqueous isopropanol of lead solution and iodine methylamine；Then, the isopropanol that MAI is added dropwise during spin coating iodate lead solution is molten
Liquid can control the crystalline condition of perovskite thin film, most by controlling the dripping quantity of the aqueous isopropanol of MAI and opportunity being added dropwise
The perovskite thin film that large area is smooth, pin-free is obtained eventually.
2, the perovskite thin film of high quality has been obtained on hackly mesoporous substrate using method provided by the invention,
Perovskite thin film surfacing obtained is fine and close, and pin-free, crystallite dimension greatly reduces carrier in crystal boundary up to a few micrometers
The loss at place is conducive to application of the perovskite material in photoelectric field.
Description of the drawings
Fig. 1 is the SEM figures for the perovskite thin film that comparative example 1 (a), comparative example 2 (b) and embodiment 1 (c) obtain；
Fig. 2 is pure lead iodide films, and after iodate lead solution spin coating 0s, 5s, 10s, 15s, 20s, 25s, 30s,
The SEM figures for the perovskite thin film that the aqueous isopropanol of dropwise addition iodine methylamine obtains；
Fig. 3 is the X ray diffracting spectrum for the perovskite thin film that comparative example 1, comparative example 2 and embodiment 1 obtain.
Specific implementation mode
With reference to the accompanying drawings and examples, technical scheme of the present invention is described in detail.
A method of perovskite thin film is prepared based on anti-solvent dynamic spin coating, specifically includes following steps：
Step 1, cleaning substrate：
The FTO electro-conductive glass of having electronic transport layer is cleaned by ultrasonic 20min by 1.1 respectively in acetone, alcohol, water successively,
It is dried in vacuum drying chamber；
The FTO electro-conductive glass of 1.2 pairs of upper steps treated having electronic transport layer carries out UV-ozone processing, to increase lining
The hydrophily at bottom；
Step 2 using lead iodide as solute, organic solvent is solvent, stirring and dissolving, preparation obtain mass concentration be 0.3~
The iodate lead solution of 0.6g/mL；With iodine methylamine (CH3NH3I, MAI) it is used as solute, isopropanol as solvent, stirring and dissolving is prepared
Obtain the aqueous isopropanol for the iodine methylamine that mass concentration is 30~70mg/mL；
The iodate lead solution that step 2 is prepared is placed on heating stirring platform, the pre-heat treatment 10 at 60~70 DEG C by step 3
~15min；
Step 4 forms perovskite thin film using spin-coating method on the substrate after step 1 is cleaned, and spin coating rotating speed is
3000rpm, time 30s；Detailed process is：First, on the substrate that step 1 cleans up after 3 the pre-heat treatment of a dropping step
Iodate lead solution, start spin coating；The aqueous isopropanol for the iodine methylamine that a dropping step 2 is prepared after 5~25s of spin coating continues spin coating,
Wherein, the volume ratio of iodate lead solution and the aqueous isopropanol of iodine methylamine is (0.6~1.6)：1；During continuing spin coating, iodine
The aqueous isopropanol of methylamine reacted with lead iodide generate perovskite, at 150 DEG C toast 10~60min, removal residual solution and
Surface layer excess MAI, you can obtain perovskite thin film.
Further, step 2 to step 4 is carried out in the glove box of nitrogen atmosphere.
Further, when step 4 uses spin-coating method to form perovskite thin film on the substrate after step 1 cleaning, acceleration
For 1000rpm/s.
Embodiment 1
A method of perovskite thin film is prepared based on anti-solvent dynamic spin coating, specifically includes following steps：
Step 1, cleaning substrate：
1.1 will be with TiO2The FTO electro-conductive glass of electron transfer layer is cleaned by ultrasonic in acetone, alcohol, water respectively successively
20min is dried in vacuum drying chamber；
Treated with TiO for 1.2 pairs of upper steps2The FTO electro-conductive glass of electron transfer layer carries out at the UV-ozone of 20min
Reason, to increase the hydrophily of substrate；
Step 2 by solute, DMF of lead iodide is solvent, stirs 12h, and it is 0.416g/mL's to prepare and obtain mass concentration
Iodate lead solution；With iodine methylamine (CH3NH3I, MAI) it is used as solute, isopropanol as solvent, 12h is stirred, it is dense that preparation obtains quality
Degree is the aqueous isopropanol of the iodine methylamine of 50mg/mL；
The iodate lead solution that step 2 is prepared is placed on heating stirring platform, the pre-heat treatment 15min at 70 DEG C by step 3；
Step 4 forms perovskite thin film using spin-coating method on the substrate after step 1 is cleaned, and spin coating rotating speed is
3000rpm, time 30s, acceleration 1000rpm/s；Detailed process is：First, on the substrate that step 1 cleans up
The even iodate lead solution being added dropwise after 50 microlitres of step 3 the pre-heat treatments, starts spin coating；50 microlitres of steps 2 are added dropwise after spin coating 10s to prepare
Iodine methylamine aqueous isopropanol, continue spin coating 20s；During continuing spin coating, the aqueous isopropanol and lead iodide of iodine methylamine
Reaction generates perovskite, toasts 10min at 150 DEG C, you can obtain perovskite thin film.
Embodiment 2
Perovskite thin film is prepared according to the step of embodiment 1, sets the time for the aqueous isopropanol that MAI is added dropwise to：Rotation
After applying 0s, 5s, 15s, 20s, 25s, 30s, the aqueous isopropanol of iodine methylamine is added dropwise.The SEM for the perovskite thin film that embodiment 2 obtains
As shown in Figure 2.
Comparative example 1
Comparative example 1 is that traditional one-step method prepares perovskite thin film.Detailed process is：
(1) substrate is cleaned：
1.1 will be with TiO2The FTO electro-conductive glass of electron transfer layer is cleaned by ultrasonic in acetone, alcohol, water respectively successively
20min is dried in vacuum drying chamber；
Treated with TiO for 1.2 pairs of upper steps2The FTO electro-conductive glass of electron transfer layer carries out at the UV-ozone of 20min
Reason, to increase the hydrophily of substrate；
(2) preparation of perovskite precursor liquid：
It takes 0.2g MAI and 0.578g lead iodides to be added in 1mL DMF, 12h is stirred at 60 DEG C to solution clear,
Obtain perovskite precursor liquid；
(3) preparation of perovskite thin film：
The perovskite precursor liquid that 50 microlitres of steps (2) obtain is taken to be added dropwise on the substrate that step (1) cleans up, with
The rotating speed spin coating 30s of 3000rpm, then toasts 20min, you can obtain perovskite thin film at 100 DEG C.
Comparative example 2
Comparative example 2 is that traditional two step spin-coating methods prepare perovskite thin film.Comparative example 2 compared with Example 1, is distinguished as：Step
When forming perovskite thin film on the substrate in rapid 4 using spin-coating method after step 1 cleaning, detailed process is：First, 50 microlitres are taken
Iodate lead solution after step 3 the pre-heat treatment is added dropwise on the substrate cleaned up, after the rotating speed spin coating 30s of 3000rpm,
5min is toasted at 100 DEG C；Then after upper step, treated after substrate is cooled to room temperature, and 50 microlitres of steps 2 are added dropwise on its surface and match
The aqueous isopropanol of the iodine methylamine of system toasts 20min, you can obtain calcium after the rotating speed spin coating 30s of 3000rpm at 150 DEG C
Titanium ore film.
As shown in Figure 1, the SEM figures of the perovskite thin film obtained for comparative example 1 (a), comparative example 2 (b) and embodiment 1 (c)；
As shown in Figure 1, the perovskite thin film surfacing that embodiment 1 obtains is fine and close, and pin-free, crystallite dimension can reach 1.86 microns.
As shown in Fig. 2, be pure lead iodide films, and iodate lead solution spin coating 0s, 5s, 10s, 15s, 20s, 25s,
After 30s, the SEM figures of the obtained perovskite thin film of aqueous isopropanol of iodine methylamine are added dropwise, reflect the drop of the aqueous isopropanol of MAI
Influence of the added-time machine to perovskite thin film obtained.As shown in Figure 2, the aqueous isopropanol of MAI is added dropwise on different opportunitys, obtains
The surface topography of perovskite thin film differ greatly, the basic variation tendency that spininess pore membrane-flatted membrane-grain films fine crushing are presented,
The film morphology that the aqueous isopropanol of dropwise addition MAI obtains after spin coating 10s is optimal.
As shown in figure 3, the X ray diffracting spectrum of the perovskite thin film obtained for comparative example 1, comparative example 2 and embodiment 1.
From the figure 3, it may be seen that pure phase perovskite structure is presented in the perovskite thin film that embodiment 1 obtains, the impurity such as no lead iodide remain, compared to
The film that comparative example 1 and comparative example 2 obtain, diffraction peak intensity is most strong, halfwidth is minimum, and crystalline quality is best.
A kind of method preparing perovskite thin film based on anti-solvent dynamic spin coating provided by the invention, efficiently solves tradition
The film spininess hole that one step spin-coating method the obtains problem small with the film crystal grain that traditional two step spin-coating methods obtain, passes through anti-solvent
(isopropanol) Rapid Extraction lead iodide, and reacted with the MAI dissolved in anti-solvent and generate perovskite crystal, finally rough
Mesoporous substrate on obtained the perovskite thin film of high quality.
Claims (5)
1. a kind of method preparing perovskite thin film based on anti-solvent dynamic spin coating, includes the following steps：
Step 1, cleaning substrate；
Step 2 by solute, organic solvent of lead iodide is solvent, and it is molten to prepare the lead iodide that mass concentration is 0.3~0.6g/mL
Liquid；Using iodine methylamine as solute, isopropanol as solvent, the isopropanol for the iodine methylamine that mass concentration is 30~70mg/mL is prepared
Solution；
Step 3, the iodate lead solution for preparing step 2 10~15min of the pre-heat treatment at 60~70 DEG C；
Step 4 forms perovskite thin film using spin-coating method on the substrate after step 1 is cleaned, and spin coating rotating speed is 3000rpm, when
Between be 30s；Detailed process is：First, the lead iodide on the substrate that step 1 cleans up after 3 the pre-heat treatment of a dropping step is molten
Liquid starts spin coating；The aqueous isopropanol for the iodine methylamine that a dropping step 2 is prepared after 5~25s of spin coating continues spin coating, wherein iodate
The volume ratio of lead solution and the aqueous isopropanol of iodine methylamine is (0.6~1.6)：1；After spin coating, toasted processing obtains calcium
Titanium ore film.
2. the method according to claim 1 for preparing perovskite thin film based on anti-solvent dynamic spin coating, which is characterized in that step
Rapid 1 substrate is the electro-conductive glass of having electronic transport layer.
3. the method according to claim 1 for preparing perovskite thin film based on anti-solvent dynamic spin coating, which is characterized in that step
Rapid 2 organic solvent is the mixed solvent of DMF, DMSO or DMF and DMSO.
4. the method according to claim 1 for preparing perovskite thin film based on anti-solvent dynamic spin coating, which is characterized in that step
Rapid 2 to step 4 carried out in the glove box of nitrogen atmosphere.
5. the method according to claim 1 for preparing perovskite thin film based on anti-solvent dynamic spin coating, which is characterized in that step
Rapid 4 use spin-coating method on the substrate after step 1 cleaning when formation perovskite thin film, acceleration 1000rpm/s.
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| CN109768166A (en) * | 2019-01-16 | 2019-05-17 | 深圳市前海首尔科技有限公司 | A kind of perovskite solar battery and preparation method thereof |
| CN109904319A (en) * | 2019-01-29 | 2019-06-18 | 安徽大学 | The flat crystal of large scale perovskite, calcium titanium ore bed preparation method and solar battery |
| CN109950397A (en) * | 2019-01-16 | 2019-06-28 | 深圳市前海首尔科技有限公司 | A kind of preparation process of high performance calcium titanium ore solar battery thin film |
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| CN112968132A (en) * | 2019-12-13 | 2021-06-15 | 中国科学院大连化学物理研究所 | Preparation method of perovskite battery |
| US11282700B2 (en) | 2019-04-17 | 2022-03-22 | University Of Kentucky Research Foundation | Method for manufacturing perovskite-based devices in ambient air |
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| CN111200065B (en) * | 2018-11-19 | 2022-09-02 | 杭州纤纳光电科技有限公司 | Method for preparing perovskite solar cell |
| CN109638162A (en) * | 2018-12-14 | 2019-04-16 | 江西理工大学 | A kind of high quality CsPbI2The preparation method of the inorganic perovskite thin film of Br |
| CN109638162B (en) * | 2018-12-14 | 2022-07-05 | 江西理工大学 | High-quality CsPbI2Preparation method of Br inorganic perovskite film |
| CN109768166A (en) * | 2019-01-16 | 2019-05-17 | 深圳市前海首尔科技有限公司 | A kind of perovskite solar battery and preparation method thereof |
| CN109950397A (en) * | 2019-01-16 | 2019-06-28 | 深圳市前海首尔科技有限公司 | A kind of preparation process of high performance calcium titanium ore solar battery thin film |
| CN109904319A (en) * | 2019-01-29 | 2019-06-18 | 安徽大学 | The flat crystal of large scale perovskite, calcium titanium ore bed preparation method and solar battery |
| CN109904319B (en) * | 2019-01-29 | 2022-11-18 | 安徽大学 | Preparation method of large-size perovskite flat crystal and perovskite layer and solar cell |
| US11282700B2 (en) | 2019-04-17 | 2022-03-22 | University Of Kentucky Research Foundation | Method for manufacturing perovskite-based devices in ambient air |
| CN110098332A (en) * | 2019-04-25 | 2019-08-06 | 华南理工大学 | A kind of preparation method for the perovskite thin film being suitable for a high-humidity environment |
| CN112968132A (en) * | 2019-12-13 | 2021-06-15 | 中国科学院大连化学物理研究所 | Preparation method of perovskite battery |
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