CN107118110B - A method of perovskite CH3NH3PbI3 film is prepared with transverse current - Google Patents
A method of perovskite CH3NH3PbI3 film is prepared with transverse current Download PDFInfo
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- CN107118110B CN107118110B CN201710329087.0A CN201710329087A CN107118110B CN 107118110 B CN107118110 B CN 107118110B CN 201710329087 A CN201710329087 A CN 201710329087A CN 107118110 B CN107118110 B CN 107118110B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/24—Lead compounds
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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
- H10K71/125—Deposition of organic active material using liquid deposition, e.g. spin coating using electrolytic deposition e.g. in-situ electropolymerisation
Abstract
Perovskite CH is prepared with transverse current the invention discloses a kind of3NH3PbI3The method of film, this method is in perovskite CH3NH3PbI3After precursor liquid room temperature scratches, electrode is placed in the perovskite CH at substrate both ends3NH3PbI3On precursor liquid, perovskite CH is given using constant-current supply3NH3PbI3Precursor liquid is powered, and makes perovskite CH3NH3PbI3Precursor liquid crystallizes under the action of electric current, and perovskite CH can be obtained3NH3PbI3Film.Operation of the present invention is simple, and knifing process does not need to heat, and only need to apply electric current can make perovskite CH3NH3PbI3Precursor liquid rapid crystallization does not need to anneal after blade coating yet, reduce the production cost.
Description
Technical field
The invention belongs to perovskite thin film manufacture technology fields, and in particular to one kind is preparing perovskite CH3NH3PbI3It is thin
The method for making perovskite room temperature that electric current be added to crystallize in membrane process.
Background technique
Perovskite material has become one of the hot spot of material science research field in recent years, due to current-carrying with higher
The advantages that transport factor, strong light absorpting ability, higher luminous efficiency, diffusion length length, low manufacture cost, cause to close extensively
Note.It can be applicable to electronic device and opto-electronic device etc., such as perovskite light emitting diode, photodetector, solar energy
Battery etc..There are many perovskite thin film preparation method at present, such as: solwution method, double source coevaporation method, successive sedimentation method and steam
Assisted solution method etc..But these method manufacture crafts are more complex, controllable factor is more, made device it is less reproducible, and
And require annealing steps.As solwution method be first by the spin coating of perovskite precursor liquid on substrate, it is then further that perovskite is thin
Film is in high-purity N2It anneals 10 minutes for 100 DEG C in the glove box of atmosphere, perovskite thin film is made further to crystallize and grow up.However in hand
Casing N2It anneals in atmosphere, increases cost of manufacture.
Summary of the invention
It is an object of the invention to solve to be needed in above-mentioned solwution method by perovskite CH3NH3PbI3Film is in glove box N2Atmosphere
The problem of middle annealing, provides one kind and does not need to anneal, directly makes perovskite CH in air3NH3PbI3Precursor liquid rapid crystallization system
Standby perovskite CH3NH3PbI3The method of film.
Solving technical solution used by above-mentioned technical problem is: by perovskite CH3NH3PbI3Forerunner's drop is dry in cleaning
On net FTO electro-conductive glass, and room temperature blade coating is carried out with blade coating instrument；After blade coating, electrode is placed in FTO electro-conductive glass both ends
Perovskite CH3NH3PbI3On precursor liquid, perovskite CH is given using constant-current supply3NH3PbI3Precursor liquid is powered, and supply voltage is
10~20V, size of current are 3~9mA, and conduction time is to obtain perovskite CH in 30~60 seconds3NH3PbI3Film.
In the above method, optimization power supply voltage is 10~20V, size of current is 5~7mA, and conduction time is 30~60 seconds.
Above-mentioned perovskite CH3NH3PbI3Precursor liquid is by CH3NH3I and PbI2Dimethyl methyl is added for 1:1 in molar ratio
In amide, the CH of 1.0 obtained~1.5mol/L3NH3PbI3Solution.
The present invention is in perovskite CH3NH3PbI3After precursor liquid room temperature scratches, electrode is placed in the calcium titanium at substrate both ends
Mine CH3NH3PbI3On precursor liquid, perovskite CH is given using constant-current supply3NH3PbI3Precursor liquid is powered, and makes perovskite CH3NH3PbI3
Precursor liquid crystallizes under the action of electric current, and perovskite CH can be obtained3NH3PbI3Film.Operation of the present invention is simple, knifing process
It does not need to heat, only need to apply electric current can make perovskite CH3NH3PbI3Precursor liquid rapid crystallization does not need to move back after blade coating yet
Fire reduces the production cost.
Detailed description of the invention
Fig. 1 is that the function of current prepares perovskite CH3NH3PbI3The apparatus structure schematic diagram of film 1 is glass substrate in figure,
2 it is FTO conductive layer, 3 is perovskite CH3NH3PbI3Precursor liquid, 4 be electrode, 5 be ammeter, 6 be constant-current supply.
Fig. 2 be constant-current supply voltage be 14V, the perovskite CH for preparing when size of current is 3.94mA3NH3PbI3Film
XRD diffraction pattern.
Fig. 3 be constant-current supply voltage be 14V, the perovskite CH for preparing when size of current is 4.96mA3NH3PbI3Film
XRD diffraction pattern.
Fig. 4 be constant-current supply voltage be 14V, the perovskite CH for preparing when size of current is 5.92mA3NH3PbI3Film
XRD diffraction pattern.
Fig. 5 be constant-current supply voltage be 14V, the perovskite CH for preparing when size of current is 6.95mA3NH3PbI3Film
XRD diffraction pattern.
Fig. 6 be constant-current supply voltage be 14V, the perovskite CH for preparing when size of current is 7.93mA3NH3PbI3Film
XRD diffraction pattern.
Fig. 7 is perovskite CH3NH3PbI3The mean intensity of crystal face (110), (220) and (310) diffraction maximum.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention is not limited only to
These embodiments.
Embodiment 1
After FTO electro-conductive glass having a size of 2.5cm × 2.5cm is wiped with dehydrated alcohol, dehydrated alcohol, third are successively used
Ketone, isopropanol, dehydrated alcohol are respectively cleaned by ultrasonic 30mins, removal surface organic matter residual.By 0.3816g (0.0024mol)
CH3NH3I and 1.1064g (0.0024mol) PbI2It is added in 2mL dimethylformamide, stirring to solution is clarified, and is obtained
The CH of 1.2mol/L3NH3PbI3Solution, i.e. perovskite CH3NH3PbI3Precursor liquid.As shown in Figure 1, taking perovskite with liquid-transfering gun
CH3NH3PbI340 μ L of precursor liquid drips on the FTO electro-conductive glass after above-mentioned cleaning and carries out room temperature blade coating with blade coating instrument, is arranged
Blade coating speed is 1000mm/min.After blade coating, electrode is placed in the perovskite CH at FTO electro-conductive glass both ends3NH3PbI3Before
It drives on liquid, gives perovskite CH using constant-current supply3NH3PbI3Precursor liquid is powered, and supply voltage 14V, size of current are
3.94mA, conduction time are 40 seconds, obtain perovskite CH3NH3PbI3Film.As shown in Fig. 2, being 14 °, 28 ° and 32 ° in angle
There is perovskite CH in place3NH3PbI3Crystal face (110), (220) and (310) diffraction maximum, relative intensity is respectively 80,140,
50。
Embodiment 2
In the present embodiment, supply voltage 14V, size of current 4.96mA, other conditions are same as Example 1, obtain
Perovskite CH3NH3PbI3Film.As shown in figure 3, being perovskite CH occur at 14 °, 28 ° and 32 ° in angle3NH3PbI3Crystal face
(110), the diffraction maximum of (220) and (310), relative intensity are respectively 130,150,90.
Embodiment 3
In the present embodiment, supply voltage 14V, size of current 5.92mA, other conditions are same as Example 1, obtain
Perovskite CH3NH3PbI3Film.As shown in figure 4, there is perovskite CH when angle is 14 °, 28 ° and 32 °3NH3PbI3Crystal face
(110), the diffraction maximum of (220) and (310), relative intensity are respectively 140,150,70.
Embodiment 4
In the present embodiment, supply voltage 14V, size of current 6.95mA, other conditions are same as Example 1, obtain
Perovskite CH3NH3PbI3Film.As shown in figure 5, there is perovskite CH when angle is 14 °, 28 ° and 32 °3NH3PbI3Crystal face
(110), the diffraction maximum of (220) and (310), relative intensity are respectively 250,225,60.
Embodiment 5
In the present embodiment, supply voltage 14V, size of current 7.93mA, other conditions are same as Example 1, obtain
Perovskite CH3NH3PbI3Film.As shown in fig. 6, there is perovskite CH when angle is 14 °, 28 ° and 32 °3NH3PbI3Crystal face
(110), the diffraction maximum of (220) and (310), relative intensity are respectively 160,150,70.
Illustrated by the XRD characterization result of above-mentioned Fig. 2~6, perovskite CH3NH3PbI3Precursor liquid can be fast under the function of current
Speed crystallization, forms perovskite CH3NH3PbI3Film.As seen from Figure 7, perovskite active layer CH when electric current is less than 3mA3NH3PbI3
Substantially it does not crystallize, when size of current is 3mA~7mA, with the increase perovskite CH of electric current3NH3PbI3The crystallinity of film becomes
It is good, and since electric current is excessive when electric current is 7mA~9mA, the crystallization of perovskite can be deteriorated again.Therefore the present invention passes through transverse current
Method can control the crystallinity of perovskite thin film.
Claims (2)
1. a kind of prepare perovskite CH with transverse current3NH3PbI3The method of film, it is characterised in that: by perovskite
CH3NH3PbI3Forerunner's drop carries out room temperature blade coating on the FTO electro-conductive glass cleaned up, and with blade coating instrument；After blade coating,
Electrode is placed in the perovskite CH at FTO electro-conductive glass both ends3NH3PbI3On precursor liquid, using constant-current supply to perovskite
CH3NH3PbI3Precursor liquid is powered, and supply voltage is 10~20V, size of current is 5~7mA, and conduction time is 30~60 seconds, obtains
To perovskite CH3NH3PbI3Film.
2. according to claim 1 prepare perovskite CH with transverse current3NH3PbI3The method of film, it is characterised in that:
The perovskite CH3NH3PbI3Precursor liquid is by CH3NH3I and PbI2It is added in dimethylformamide, obtains for 1:1 in molar ratio
The CH of the 1.0~1.5mol/L arrived3NH3PbI3Solution.
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| CN110518130B (en) * | 2019-08-28 | 2021-01-01 | 上海交通大学 | Method for regulating secondary growth of perovskite crystal grains by electric field |
| CN113862712B (en) * | 2021-09-15 | 2023-12-01 | 中山大学 | Preparation method of lead-containing or bismuth-containing perovskite nanocrystals |
| CN115036430A (en) * | 2022-08-09 | 2022-09-09 | 中国华能集团清洁能源技术研究院有限公司 | Method for preparing perovskite film with assistance of external electric field and photoelectric device |
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