CN109449295A - Method for preparing perovskite film based on two-step printing - Google Patents
Method for preparing perovskite film based on two-step printing Download PDFInfo
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- CN109449295A CN109449295A CN201811276859.XA CN201811276859A CN109449295A CN 109449295 A CN109449295 A CN 109449295A CN 201811276859 A CN201811276859 A CN 201811276859A CN 109449295 A CN109449295 A CN 109449295A
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- 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
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
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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
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- 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
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
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- 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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Abstract
The invention relates to a method for preparing a perovskite thin film based on two-step printing, which comprises the following three steps: 1) printing and coating a perovskite inorganic component solution on the surface of a substrate, and then carrying out vacuum treatment and annealing to obtain an inorganic component film; 2) printing and coating an organic component on the inorganic component film, and reacting to obtain a perovskite intermediate phase; 3) and annealing the perovskite intermediate phase to obtain the perovskite thin film. The method can fully extract excessive solvent in the liquid film by performing vacuum treatment on the coated inorganic component, promote uniform generation of inorganic component crystal nuclei, and obtain the inorganic component film with good crystallinity, bright surface and mesoporous structure.
Description
Technical field
The invention belongs to optoelectronic film preparation and technical field of solar cells, and in particular to one kind is based on two-step method printing system
The method of standby perovskite thin film.
Background technique
Current energy shortage and combusts fossil energy bring environmental problem restrict social sustainable development, using too
It is one of the effective means for alleviating current energy and environment crisis that sun, which can generate electricity,.Perovskite solar cell is to grow up in recent years
Novel thin film solar cell.As a kind of high efficiency solar cell that can process preparation by simple solution, receive complete
The research boom of world's photovoltaic art.The efficiency for the small area perovskite battery that current experiment room is prepared based on spin coating proceeding is
Reach 23.2%.However since film is uneven when the defect of spin coating proceeding itself be easy to cause large area to prepare and material
Utilization rate is low, therefore spin coating proceeding can not be applied to the preparation of large area perovskite thin film, seriously hinders the production of perovskite battery
Industry process.
The liquid phase preparation process of perovskite can be divided into one-step method and two-step method: one-step method is by the inorganic component of perovskite
It mixes to form precursor solution with organic component, be prepared after film using film crystallization means；Two-step method
It is first to deposit inorganic component using liquid phase method, and then deposit organic component on inorganic component surface, makes two components in certain item
It is reacted under part, ultimately generates perovskite.
Commercialized printing technology theoretically can be used in perovskite solar cell, and (for example blade coating, slit squeeze out, ink-jet beats
Print etc.) carry out the continuous preparation of high speed.Have the report on a small quantity about printing technology preparation large area perovskite thin film in document,
The one-step preparation process that wherein most uses is to pass through print using the organic component of perovskite and inorganic component as presoma
Dataller's skill is coated at high temperature prepares perovskite.Since the underlayer temperature in coating process is up to 100-150 DEG C, close to molten
The boiling point of agent, therefore unavoidably cause solvent volatilization and two processes of perovskite crystalline simultaneously or intersect to carry out, thus can not
The macro-uniformity of the crystal quality of accuracy controlling perovskite, microscopic appearance and film.
During preparing perovskite using printing technology (such as scraper and slit extrusion coated technology) based on two-step method,
If the perovskite inorganic component deposited to the first step is without any processing or directly carries out to the inorganic component liquid film of coating
Annealing, will be unable to obtain the inorganic component film that crystallinity is good, surface-brightening is smooth, finally be unable to get satisfaction preparation
The perovskite photoactive film that solar cell requires.That reports on a small quantity prepares perovskite technique using printing technology based on two step method
In, in first step inorganic component deposition, it is dried using liquid film of the nitrogen air knife to deposition, to regulate and control inorganic component
Film quality.The use of nitrogen air knife can cause the film forming of inorganic component uneven due to the difference of air quantity, also increase simultaneously
Preparation cost.Therefore exploitation is new carries out perovskite thin film based on two-step process and suitable for large area printing technology
The continuous preparation of high speed has very important practical significance.
Summary of the invention
The purpose of the present invention is overcome that mentions in background above technology to prepare perovskite thin film work based on two-step method printing
The deficiency of skill provides a kind of new preparation process, that is, provides a kind of method for preparing perovskite thin film based on two-step method printing.
The purpose of the present invention is realized by following scheme:
A method of perovskite thin film is prepared based on two-step method printing, comprising the following three steps:
1) printing of perovskite inorganic component solution is coated on matrix surface, is then vacuum-treated and anneals to obtain nothing
Machine component film；
2) organic component printing is coated on the inorganic component film, perovskite interphase is obtained after reaction；
3) the perovskite interphase is annealed to obtain the perovskite thin film.
The method carries out low vacuum treatment by the inorganic component liquid film that deposits to the first step, obtain crystallinity it is good,
The inorganic component film of surfacing light；And it is sufficiently anti-to carry out two components in the deposition process of second step organic component
Answer, then further annealing makes its sufficient crystallising, finally obtain crystallinity is high, film thickness uniformly, the calcium titanium in dense non-porous hole
Mine polycrystal film.This method is particularly suitable for the preparation to large area perovskite thin film.
It can be used printing technology commonly used in the art by perovskite inorganic component solution coating in matrix surface in step 1),
Including but not limited to blade coating, slit extrusion, inkjet printing, spraying and bar coating etc. printing technologies.
Preferably, the solution of perovskite inorganic component described in step 1) is PbX2Solution or PbX2- CsY solution, wherein X and Y
Respectively one or both of I, Br, the PbX2CsY and PbX in-CsY solution2Molar ratio be (0-1): 4；Perovskite without
The concentration of machine component solution is 0.5-1.5mol/L, coating speed 1-50mm/s.
Preferably, the solvent that the solution of perovskite inorganic component described in step 1) uses is the one or both of DMF, DMSO
Mixed solvent, coating temperature are 10-40 DEG C.
Preferably, vacuum processing vacuum degree described in step 1) is 1 × 10-2-1×103Pa, vacuum retention time are 10s-
10min.The solvent in inorganic component liquid film is extracted by vacuumizing, supersaturated solution is formed and is crystallized, obtained
The inorganic component film of non-sufficient crystallising.
Preferably, annealing temperature described in step 1) is 40 DEG C -100 DEG C, annealing time 5s-60min.Pass through the annealing
Processing can make remaining solvent in liquid film sufficiently volatilize, and obtain the good inorganic component film of crystallinity.
Preferably, the solution of perovskite organic component described in step 2) is MAxFA1-xY, wherein MA is CH3NH3, FA HC
(NH2)2, any number of the x between 0-1, Y is at least one of I and Br；The concentration of the perovskite organic component solution
For 20-70mg/mL, coating speed 5-50mm/s, coating temperature is 25-70 DEG C.
Preferably, annealing temperature described in step 3) is 80-200 DEG C, annealing time 1min-60min.Pass through the annealing
Crystallinity height can be obtained in processing, and film thickness is uniform, the perovskite polycrystal film in continuous needleless hole.
The perovskite thin film of two-step method preparation of the present invention can be applied to the preparation of perovskite solar cell component.
Relative to prior art technology, the invention has the following advantages:
During the present invention is for perovskite is prepared using printing technology for coating based on two-step method, caused using nitrogen air knife
Inorganic component crystalline property difference and the non-uniform disadvantage of forming a film provide a kind of technique based on vacuum aided crystallization and prepare calcium titanium
Mine inorganic component.By being vacuum-treated to the inorganic component of coating, excessive solvent in liquid film can be sufficiently extracted, promotes nothing
The uniform generation of machine component nucleus obtains good crystallinity, surface-brightening and the inorganic component film with meso-hole structure.It should
The advantage of meso-hole structure is: during second step deposits organic component, organic component can be fully infiltrated into no unit
The inside and bottom divided finally obtain pure crystal phase, surface-brightening, thickness uniformly simultaneously so that two components be made sufficiently to be reacted
And the high quality perovskite thin film in dense non-porous hole.This method is suitable for large area high speed printing technology, and perovskite may be implemented
The high speed of film is continuously prepared, and has the application potential of exploitation large area perovskite solar cell module.
Detailed description of the invention
Fig. 1 is two-step process flow chart of the present invention.
Fig. 2 is the PbI obtained with meso-hole structure of embodiment 12Film SEM figure, wherein amplification factor is 40,000 times.
Fig. 3 is MAPbI made from embodiment 13The SEM of perovskite polycrystal film schemes, and wherein amplification factor is 40,000 times.
Fig. 4 is MAPbI made from embodiment 13The perovskite solar cell that perovskite thin film is prepared as photoelectric active layer
Current -voltage curve figure.
Fig. 5 is large area MAPbI made from embodiment 13Perovskite thin film.
Fig. 6 is large area MAPbI made from example 13The UV-Visible absorption figure of perovskite thin film.
Fig. 7 is that the PbI with acicular texture is made in embodiment 22The SEM of-CsI film schemes, and wherein amplification factor is 40,000
Times.
Fig. 8 is that MA is made in embodiment 20.9Cs0.1PbI3The SEM of perovskite polycrystal film schemes, and wherein amplification factor is 40,000
Times.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings.
By taking scraper film as an example, process flow of the invention is as shown in Figure 1.
Embodiment 1
Small area (2.5 × 2.5cm2) and large area perovskite thin film (9.5 × 8cm2) and corresponding solar cell system
It is standby:
1) use DMSO:DMF=9:1 as mixed solvent, compound concentration is the PbI of 461mg/mL2Solution uses scraper
Technology for coating is in one layer of PbI of electroconductive ITO substrate coated thereon2, obtained PbI2Liquid film, color are faint yellow；Wherein scraper with
Height between ITO substrate is 150 microns, uses (2.5 × 2.5cm when small area substrate2) PbI2Solution usage is 25 μ L,
Use (9.5 × 8cm when large-area substrates2) PbI2Solution usage is 200 μ L, and the mobile speed of scraper is 10mm/s, coated heat
The temperature of platform is 25 DEG C of room temperature.
2) by the PbI of coating2Liquid film is placed in vacuum chamber, carries out vacuum pumping to chamber, holding chamber pressure is
800Pa, pressure maintaining 60 seconds in this vacuum environment, most of solvent in liquid film flees from liquid film forming supersaturated solution at this time,
Obtain the PbI of glassy yellow2Crystal film.Then to the PbI2Crystal film does annealing at 70 DEG C 3 minutes, thin to remove
Remaining solvent in film.Vacuum processing can sufficiently extract excessive solvent in liquid film, promote the uniform generation of inorganic component nucleus,
As shown in Fig. 2, the PbI observed under the electronic scanner microscope of magnification at high multiple2For sheet porous structural, this meso-hole structure has
Help the infiltration of organic component.
3) using isopropanol as solvent, using doctor blade process by the MAI solution coating of 50mg/mL in PbI2On surface, scrape
Height between heel ITO substrate is 150 microns, uses small area substrate (2.5 × 2.5cm2) when MAI solution usage be 50
μ L uses large-area substrates (9.5 × 8cm2) MAI solution usage be 300 μ L, the mobile speed of scraper is 15mm/s.Coating
The temperature of thermal station is 50 DEG C, makes MAI and PbI2It is sufficiently reacted, then gained film is placed in 100 DEG C of thermal station and is annealed
10min obtains MAPbI3Perovskite thin film, with a thickness of 400nm.As shown in figure 3, under the electronic scanner microscope of magnification at high multiple
Observe obtained MAPbI3Film is continuous needleless hole, perovskite polycrystal film of the crystallite dimension in 1 microns.
4) perovskite thin film surface is rinsed using isopropanol, to remove the excessive unreacted organic component in surface
MAI。
Perovskite thin film preparation structure obtained by use is Glass/ITO/PEDOT/MAPbI3The calcium titanium of/PCBM/BCP/Ag
Mine solar cell.Small area battery (the effective area 0.09cm2) can obtain 14% or so incident photon-to-electron conversion efficiency,
Fig. 4 show the current-voltage characteristic curve of prepared battery.
Fig. 5 show large area (9.5 × 8cm based on two-step method blade coating preparation2)MAPbI3Perovskite thin film.It can by Fig. 6
See, by detecting the film in the average transmittance (400-800nm) of different location, it can be found that the uniformity of film is 95%
More than.
Embodiment 2
Small area (2.5 × 2.5cm2)MA0.9Cs0.1PbI3The preparation of perovskite thin film:
1) it uses DMSO:DMF=1:1 as mixed solvent, prepares PbI2With CsI concentration be respectively 461mg/mL and
The mixed solution of 26mg/mL is coated with one layer of mixed solution in conductive FTO substrates using scraper technology for coating, obtains
PbI2- CsI liquid film color is faint yellow.Wherein scraper is 150 microns with the height between ITO substrate, PbI2Solution usage is
25 μ L, the mobile speed of scraper are 10mm/s, and the temperature for being coated with thermal station is 25 DEG C of room temperature.
2) by the PbI of coating2- CsI liquid film is placed in vacuum chamber, is carried out vacuum pumping to chamber, is kept chamber pressure
Power is 500Pa, pressure maintaining 30 seconds in this vacuum environment, and most of solvent flees from liquid film forming supersaturated solution in liquid film at this time,
Obtain the PbI of glassy yellow2- CsI crystal film.To the PbI of vacuum processing2- CsI makes annealing treatment 10 minutes at 60 DEG C, with removal
Remaining solvent in film.As shown in fig. 7, the PbI observed under the electronic scanner microscope of magnification at high multiple2- CsI is needle-shaped
Meso-hole structure, this meso-hole structure facilitate the infiltration of organic component.
3) using isopropanol as solvent, using doctor blade process by the MAI solution coating of 40mg/mL in PbI2The surface-CsI
On, scraper is 150 microns with the height between ITO substrate, and MAI solution usage is 50 μ L, and the mobile speed of scraper is 15mm/s.
The temperature for being coated with thermal station is 55 DEG C, makes organic component MAI and inorganic component PbI2- CsI is sufficiently reacted, and then at 100 DEG C
Carry out annealing 5min and obtain the good perovskite thin film of crystallinity, film with a thickness of 400 nanometers.It is swept in the electronics of magnification at high multiple
Retouch the MA observed under microscope0.9Cs0.1PbI3For continuous needleless hole, perovskite polycrystalline of the crystallite dimension in 200 rans
Film, as shown in Figure 8.
Embodiment 3
Small area (2.5 × 2.5cm2)MAPbI2.7Br0.3The preparation of perovskite thin film:
Referring to the preparation method of perovskite thin film in embodiment 1, the difference is that inorganic component used in step 1)
For the PbI of total concentration 1M2-PbBr2(molar ratio 0.9:0.1), solvent DMF:DMSO=6:4.
Embodiment 4
Small area (2.5 × 2.5cm2)FA0.9Cs0.1PbI3The preparation of perovskite thin film:
Referring to the preparation method in embodiment 2, the difference is that substituting MAI, the concentration of FAI using FAI in step 3)
For 100mg/mL, and coating temperature is 60 DEG C.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention
Technical spirit any simple modification, change and equivalent structure transformation to the above embodiments, still fall within skill of the present invention
In the protection scope of art scheme.
Claims (7)
1. a kind of method for preparing perovskite thin film based on two-step method printing, which comprises the following steps:
1) printing of perovskite inorganic component solution is coated on matrix surface, is then vacuum-treated and anneals to obtain no unit
Divide film；
2) organic component printing is coated on the inorganic component film, perovskite interphase is obtained after reaction；
3) the perovskite interphase is annealed to obtain the perovskite thin film.
2. a kind of method for preparing perovskite thin film based on two-step method printing according to claim 1, which is characterized in that step
It is rapid 1) described in perovskite inorganic component solution be PbX2Solution or PbX2- CsY solution, wherein X and Y is respectively one in I, Br
Kind or two kinds, the PbX2CsY and PbX in-CsY solution2Molar ratio be (0-1): 4；The perovskite inorganic component solution
Concentration is 0.5-1.5mol/L, coating speed 1-50mm/s.
3. a kind of method for preparing perovskite thin film based on two-step method printing according to claim 1, which is characterized in that step
It is rapid 1) described in perovskite inorganic component solution solvent be at least one of DMF and DMSO, coating temperature be 10-40 DEG C.
4. a kind of method for preparing perovskite thin film based on two-step method printing according to claim 1, which is characterized in that step
It is rapid 1) described in vacuum processing vacuum degree be 1 × 10-2-1×103Pa, vacuum retention time are 10s-10min.
5. a kind of method for preparing perovskite thin film based on two-step method printing according to claim 1, which is characterized in that step
It is rapid 1) described in annealing temperature be 40 DEG C -100 DEG C, annealing time 5s-60min.
6. a kind of method for preparing perovskite thin film based on two-step method printing according to claim 1, which is characterized in that step
It is rapid 2) described in perovskite organic component solution be MAxFA1-xY, wherein MA is CH3NH3, FA is HC (NH2)2, x is between 0-1
Any number, Y are at least one of I and Br；The concentration of the perovskite organic component solution is 20-70mg/mL, coating speed
Degree is 5-50mm/s, and coating temperature is 25-70 DEG C.
7. a kind of method for preparing perovskite thin film based on two-step method printing according to claim 1, which is characterized in that step
It is rapid 3) described in annealing temperature be 80-200 DEG C, annealing time 1min-60min.
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Cited By (7)
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| CN111029468A (en) * | 2019-12-06 | 2020-04-17 | 苏州威格尔纳米科技有限公司 | Preparation method and equipment of perovskite thin film and perovskite solar cell |
| CN111081880A (en) * | 2019-11-22 | 2020-04-28 | 武汉理工大学 | Intermediate phase for perovskite vapor phase growth and preparation method and application thereof |
| CN111312903A (en) * | 2020-03-04 | 2020-06-19 | 江苏集萃分子工程研究院有限公司 | Continuous preparation device and process for preparing perovskite thin film in two-step roll-to-roll mode |
| CN111403612A (en) * | 2020-03-23 | 2020-07-10 | 武汉理工大学 | Water system precursor perovskite film and preparation method and application thereof |
| CN112687804A (en) * | 2020-12-25 | 2021-04-20 | 昆山协鑫光电材料有限公司 | Method for preparing large-area perovskite thin film based on two-step method and application thereof |
| CN113745438A (en) * | 2021-07-19 | 2021-12-03 | 暨南大学 | Large-area perovskite light-emitting film and light-emitting diode thereof |
| CN115971003A (en) * | 2022-12-29 | 2023-04-18 | 王道胜 | Photovoltaic film assembly coating process |
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| CN111081880A (en) * | 2019-11-22 | 2020-04-28 | 武汉理工大学 | Intermediate phase for perovskite vapor phase growth and preparation method and application thereof |
| CN111081880B (en) * | 2019-11-22 | 2021-10-29 | 武汉理工大学 | Intermediate phase for perovskite vapor phase growth and preparation method and application thereof |
| CN111029468A (en) * | 2019-12-06 | 2020-04-17 | 苏州威格尔纳米科技有限公司 | Preparation method and equipment of perovskite thin film and perovskite solar cell |
| CN111312903A (en) * | 2020-03-04 | 2020-06-19 | 江苏集萃分子工程研究院有限公司 | Continuous preparation device and process for preparing perovskite thin film in two-step roll-to-roll mode |
| CN111403612A (en) * | 2020-03-23 | 2020-07-10 | 武汉理工大学 | Water system precursor perovskite film and preparation method and application thereof |
| CN112687804A (en) * | 2020-12-25 | 2021-04-20 | 昆山协鑫光电材料有限公司 | Method for preparing large-area perovskite thin film based on two-step method and application thereof |
| CN113745438A (en) * | 2021-07-19 | 2021-12-03 | 暨南大学 | Large-area perovskite light-emitting film and light-emitting diode thereof |
| CN115971003A (en) * | 2022-12-29 | 2023-04-18 | 王道胜 | Photovoltaic film assembly coating process |
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