CN105679936A - Lead-free perovskite film, and preparation method and application thereof - Google Patents
Lead-free perovskite film, and preparation method and application thereof Download PDFInfo
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- CN105679936A CN105679936A CN201610238703.7A CN201610238703A CN105679936A CN 105679936 A CN105679936 A CN 105679936A CN 201610238703 A CN201610238703 A CN 201610238703A CN 105679936 A CN105679936 A CN 105679936A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
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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
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
- H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
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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
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
- H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
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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
Abstract
The invention provides a lead-free perovskite film and a preparation method and an application thereof. The preparation method of the lead-free perovskite film comprises the steps of: weighing SnX2 and CH3NH3X as two evaporator sources, wherein the X is C1, Br or I; putting the two evaporator sources and a substrate into a cavity of a coevaporation device, and vacuumizing the cavity; heating SnX2 so as to enable SnX2 to evaporate and be deposited on the substrate; stopping heating SnX2, heating CH3NH3X so as to enable CH3NH3X to evaporate and be deposited on the substrate, and accomplishing a circulation of the alternate evaporation of SnX2 and CH3NH3X; accomplishing a second circulation of the alternate evaporation of SnX2 and CH3NH3X; and finally, taking the substrate out and performing an annealing process. According to the invention, the perovskite film is prepared by the organic and inorganic alternate coevaporation method, the film with high quality is obtained, the problem of lead pollution is solved, and the industrial development is realized.
Description
Technical field
The present invention relates to technical field of solar batteries, specifically a kind of unleaded perovskite thin film, its preparation method and application.
Background technology
Solar energy can be directly changed into electric energy by solaode, and owing to solar energy is inexhaustible clean energy resource, therefore solaode is that the mankind tackle energy crisis, seeks the important countermeasure of sustainable development. At present, crystal silicon solar energy battery occupies the photovoltaic market share of 89%. But, expensive raw material and loaded down with trivial details battery process thereof limit the long term growth of crystal silicon solar energy battery. In 10 years of past, thin-film solar cells includes silica-base film, Cu (In, Ga) Se2-xSxAnd CdTe battery etc. also begins to realize extensive industrialization. As the outstanding representative of third generation solar cell, perovskite solaode is a kind of novel all solid state organic metal halogenide thin-film solar cells of class producing light induced electron and hole pair with organic-inorganic perovskite material. Perovskite solaode has energy conversion efficiency height, and carrier diffusion length length, mobility are high, and the advantages such as core photoelectric conversion material is cheap and easy to get, through the development of short 5 years, its laboratory conversion efficiency was promoted to about 20.1% from 3.8%.
At present, used in perovskite solaode perovskite material is mainly lead iodide methylamine (CH3NH3PbI3), its band gap is about 1.5eV, and extinction coefficient are high, and hundreds of nanometer thickness thin film just can fully absorb the sunlight of below 800nm. CH3NH3PbI3Liquid phase one-step method is generally adopted to complete in the preparation, it may be assumed that by PbI2With CH3NH3I, with certain molar ratio mixing, is then dissolved in DMF (DMF) solution, is spun in corresponding substrate until completely dissolved, afterwards thin film is carried out heat treatment and namely form CH3NH3PbI3Perovskite thin film. But, to be observed by SEM, adopt perovskite thin film prepared by liquid phase one-step method very discontinuous, coverage is relatively low, affects the open-circuit voltage of battery. And, adopt liquid phase one-step method to prepare perovskite thin film, be unfavorable for the development of industrialization. Further, containing lead element in lead iodide methylamine, owing to lead to human body health and environmental danger, therefore can be listed in many places and prohibit the use of material.
Summary of the invention
An object of the present invention is just to provide a kind of unleaded perovskite thin film, and this unleaded perovskite thin film Sn instead of Pb, it is achieved that the development and utilization of environmentally friendly novel energy.
The preparation method that the two of the purpose of the present invention are just to provide a kind of unleaded perovskite thin film, the method adopts organic-inorganic to replace the method for coevaporation to prepare unleaded perovskite thin film, it is possible to resolve the perovskite thin film coverage prepared by existing liquid phase one-step method is low and the problem that is unfavorable for industrialized development.
The three of the purpose of the present invention are just to provide the application of a kind of above-mentioned unleaded perovskite thin film, that is: a kind of perovskite solaode is provided, this perovskite solaode applies above-mentioned unleaded perovskite thin film, so that this perovskite solaode has the advantages such as photovoltaic performance is good, environmentally friendly.
An object of the present invention is achieved in that a kind of unleaded perovskite thin film, and the chemical general formula of described unleaded perovskite thin film is CH3NH3SnX3; Wherein, X is Cl, Br or I.
Unleaded perovskite thin film provided by the present invention, is replaced the Pb in traditional perovskite thin film by Sn, it is possible to resolve because of the pollution on the environment problem containing Pb in existing perovskite thin film; And this unleaded perovskite thin film has higher quality and coverage.
The preparation method that the two of the purpose of the present invention are achieved in that a kind of unleaded perovskite thin film, comprises the steps:
A, weigh SnX2And CH3NH3X, X are Cl, Br or I;
B, the SnX that will weigh2And CH3NH3X puts into the chamber of coevaporation equipment as two evaporation sources, arranges substrate in the chamber of coevaporation equipment simultaneously;
C, chamber to coevaporation equipment carry out evacuation;
D, to SnX2Evaporation source is heated, and makes SnX2Evaporate and be deposited on substrate; Stop afterwards SnX2Evaporation source is heated, then to CH3NH3X evaporation source heats, and makes CH3NH3X evaporates and is deposited on substrate, completes SnX2And CH3NH3One circulation of X alternatively vaporised;
E, repetition step d, complete SnX2And CH3NH3Second circulation of X alternatively vaporised;
F, taking-up substrate, and be annealed processing to it, namely make unleaded perovskite thin film CH after having annealed3NH3SnX3。
Preferably, in step f, annealing temperature is 100 DEG C ~ 160 DEG C, and annealing time is 20min ~ 40min.
It is furthermore preferred that annealing temperature is 160 DEG C in step f, annealing time is 30min.
Preferably, the unleaded perovskite thin film CH formed in step f3NH3SnX3Thickness be 280nm ~ 450nm.
Preferably, the chamber of coevaporation equipment is evacuated to 5 × 10 by step c-5Pa~30×10-5Pa。
The method that the present invention replaces coevaporation by organic-inorganic prepares perovskite thin film, compares the perovskite thin film coverage prepared by existing liquid phase one-step method high; And, the present invention uses Sn to replace the Pb in tradition organic inorganic hybridization perovskite thin film, it may be achieved the preparation of environmentally friendly novel energy, also be simultaneously Sn-based(tinbase) industrialization of unleaded perovskite solaode provides a kind of possible.
Adopt the present invention not only can obtain the unleaded perovskite thin film of high quality and large size, but also the problem of lead contamination can be solved, be conducive to environmental conservation; 3rd, thin film prepared by organic-inorganic coevaporation method is more smooth, it is simple to large area produces, and the industrialization for unleaded perovskite battery provides possibility.
The three of the purpose of the present invention are achieved in that a kind of perovskite solaode, and the perovskite thin film in described perovskite solaode is unleaded perovskite thin film, and the chemical general formula of described unleaded perovskite thin film is CH3NH3SnX3; Wherein, X is Cl, Br or I.
Adopt the unleaded perovskite thin film prepared by method in the present invention, perovskite solaode can be met completely to the high-quality requirement of perovskite thin film, adopt this high-quality unleaded perovskite thin film, the perovskite solaode of efficient stable may finally be obtained.
Accompanying drawing explanation
Fig. 1 is the perovskite thin film CH of gained under different annealing temperature in the embodiment of the present invention3NH3SnI3XRD comparison diagram.
The perovskite thin film CH of gained when Fig. 2 is that in the embodiment of the present invention, annealing temperature is 160 DEG C3NH3SnI3SEM figure.
The perovskite thin film CH of gained when Fig. 3 is that in the embodiment of the present invention, annealing temperature is 160 DEG C3NH3SnI3Fluorescence spectrum figure.
Detailed description of the invention
The chemical general formula of unleaded perovskite thin film provided by the present invention is CH3NH3SnX3; Wherein, X is Cl, Br or I. The preparation method of this unleaded perovskite thin film is specific as follows:
A, weigh SnX2Powder and CH3NH3X powder, X is Cl, Br or I.
B, the SnX that will weigh2And CH3NH3X puts into the chamber of coevaporation equipment as two evaporation sources, places substrate (or claiming substrate, substrate) in the chamber of coevaporation equipment simultaneously; Coevaporation equipment can be multi-source coevaporation equipment.
C, chamber to coevaporation equipment carry out evacuation; General vacuum-pumping is to 5 × 10-5Pa~30×10-5Pa。
D, first to evaporation source SnX2It is heated, makes SnX2Evaporate and be deposited on substrate; Stop afterwards evaporation source SnX2It is heated, then to evaporation source CH3NH3X heats, and makes CH3NH3X evaporates and is deposited on substrate, completes SnX2And CH3NH3One circulation of X alternatively vaporised.
E, repetition step d, complete SnX2And CH3NH3Second circulation of X alternatively vaporised.
F, taking-up substrate, and be annealed processing to it, annealing temperature is 100 DEG C ~ 160 DEG C, and annealing time is 20min ~ 40min, namely makes unleaded perovskite thin film CH after having annealed3NH3SnX3. Unleaded perovskite thin film CH3NH3SnX3Thickness can be 280nm ~ 450nm.
Unleaded perovskite thin film provided by the present invention can apply to perovskite solaode, it is also possible to is applied to the fields such as Organic Electricity laser display (OLED).
Below in conjunction with object lesson (based on the FTO/TiO of preparation on FTO substrate2/CH3NH3SnI3The unleaded perovskite thin film of structure) describe the preparation method of unleaded perovskite thin film in the present invention in detail.
The first step: electro-conductive glass cleans and TiO2The preparation of compacted zone.
(1), FTO electro-conductive glass (being substrate, substrate or substrate) is cut to specified size (such as 10cm*10cm), in succession in deionized water, acetone, dehydrated alcohol, distinguishes ultrasonic cleaning 10min with ultrasonic cleaner afterwards, then use high-purity N2Dry up.
In other embodiments, FTO electro-conductive glass can also by the SnO of doped with fluorine2Transparent conducting glass (SnO2: F) replace.
(2), the FTO electro-conductive glass cleaned up is put in plasma processor, evacuation, and pass into oxygen, under oxygen atmosphere, process 10min.
(3), the TiO that spin coating is fine and close on the FTO electro-conductive glass handled well2Solution, is subsequently placed in Muffle furnace, makes temperature from ambient in Muffle furnace be to slowly warm up to 500 DEG C, and sinters 30min at 500 DEG C.
Fine and close TiO2The collocation method of solution is as follows:
1., measure 2.5mL dehydrated alcohol, and measure the HCl of 35 μ L2mol/L, the HCl measured is added in dehydrated alcohol, stirs;
2., measure 2.5mL dehydrated alcohol, and measure 350 μ L isopropyl titanates, the isopropyl titanate measured is added in dehydrated alcohol, stirs;
3., with pipettor aspiration step 2. in solution, and be added dropwise over step 1. in solution in, in dropping process, continuously stirred, be finally configured to densification TiO2Solution.
Second step: CH3NH3SnI3The preparation of perovskite thin film.
FTO/TiO prepared by the first step herein above2On the basis of compacted zone, in this step, first weigh a certain amount of SnI2Powder and CH3NH3Weigh two evaporation sources, as two evaporation sources, are put into the chamber of coevaporation equipment by I powder, and by the FTO/TiO of first step gained2Put into the chamber of coevaporation equipment.The chamber of coevaporation equipment is carried out evacuation, treats that vacuum is evacuated to 8 × 10-5After Pa, stop evacuation. Begin to warm up evaporation source SnI afterwards2, make SnI2Evaporate and be deposited on TiO2On compacted zone, treat film thickness gauge display deposition SnI2During to certain thickness, stop heating SnI2, heating evaporation source CH then3NH3I, equally, treats film thickness gauge display deposition CH3NH3When I is to certain thickness, stop heating CH3NH3I, now completes SnI2With CH3NH3One circulation of I alternatively vaporised. Then SnI is carried out again2With CH3NH3Second circulation of I alternatively vaporised, after completing second circulation, takes out substrate in coevaporation equipment, and recording evaporation gained thickness with step instrument is about 300nm. Anneal 30min afterwards at 100 DEG C, obtains FTO/TiO2/CH3NH3SnI3The unleaded perovskite thin film of structure. Certainly, if not adopting annealing process, but in evaporation process, substrate being heated, being also passable. Annealing and heating substrate are provided to optimize the crystallization degree of perovskite thin film.
According to above-mentioned example, changing final step annealing process condition, anneal 30min respectively at 120 DEG C, 140 DEG C, 160 DEG C and 170 DEG C, thus preparing different unleaded perovskite thin film CH3NH3SnI3。
To the unleaded perovskite thin film CH prepared by (100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C and 170 DEG C) under different annealing temperature3NH3SnI3Carrying out XRD test respectively, acquired results is shown in Fig. 1. In Fig. 1, five curves be corresponding in turn to from the bottom to top annealing temperature 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C and 170 DEG C. As seen from Figure 1, annealing temperature is in 100 DEG C to the 160 DEG C of processes raised, and along with the rising of annealing temperature, perovskite thin film crystallinity improves, and MAI(and CH3NH3X) miscellaneous peak disappears; Continuing rising along with annealing temperature or annealing time becomes big, perovskite thin film decomposes, and occurs SnI therewith2Miscellaneous peak.
Unleaded perovskite thin film CH prepared when being 160 DEG C to annealing temperature3NH3SnI3Being scanned Electronic Speculum test, acquired results is shown in Fig. 2. As seen from Figure 2, the unleaded perovskite thin film CH prepared by the present invention3NH3SnI3Crystal grain is big, coverage is high.
Unleaded perovskite thin film CH prepared when being 160 DEG C to annealing temperature3NH3SnI3Carrying out fluorescence spectrum test, acquired results is shown in Fig. 3.
The present invention adopts organic-inorganic coevaporation method to prepare unleaded perovskite thin film, is conducive to automatization, it is simple to realize industrialization, also can reduce cost simultaneously.
Claims (7)
1. a unleaded perovskite thin film, is characterized in that, the chemical general formula of described unleaded perovskite thin film is CH3NH3SnX3; Wherein, X is Cl, Br or I.
2. a preparation method for unleaded perovskite thin film, is characterized in that, comprises the steps:
A, weigh SnX2And CH3NH3X, X are Cl, Br or I;
B, the SnX that will weigh2And CH3NH3X puts into the chamber of coevaporation equipment as two evaporation sources, arranges substrate in the chamber of coevaporation equipment simultaneously;
C, chamber to coevaporation equipment carry out evacuation;
D, to SnX2Evaporation source is heated, and makes SnX2Evaporate and be deposited on substrate; Stop afterwards SnX2Evaporation source is heated, then to CH3NH3X evaporation source heats, and makes CH3NH3X evaporates and is deposited on substrate, completes SnX2And CH3NH3One circulation of X alternatively vaporised;
E, repetition step d, complete SnX2And CH3NH3Second circulation of X alternatively vaporised;
F, taking-up substrate, and be annealed processing to it, namely make unleaded perovskite thin film CH after having annealed3NH3SnX3。
3. the preparation method of unleaded perovskite thin film according to claim 2, is characterized in that, in step f, annealing temperature is 100 DEG C ~ 160 DEG C, and annealing time is 20min ~ 40min.
4. the preparation method of unleaded perovskite thin film according to claim 3, is characterized in that, in step f, annealing temperature is 160 DEG C, and annealing time is 30min.
5. the preparation method of unleaded perovskite thin film according to claim 2, is characterized in that, the unleaded perovskite thin film CH formed in step f3NH3SnX3Thickness be 280nm ~ 450nm.
6. the preparation method of unleaded perovskite thin film according to claim 2, is characterized in that, in step c, the chamber of coevaporation equipment is evacuated to 5 × 10-5Pa~30×10-5Pa。
7. a perovskite solaode, is characterized in that, the perovskite thin film in described perovskite solaode is unleaded perovskite thin film, and the chemical general formula of described unleaded perovskite thin film is CH3NH3SnX3; Wherein, X is Cl, Br or I.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106252460A (en) * | 2016-08-15 | 2016-12-21 | 常州大学 | The manufacture method of a kind of large area perovskite solaode and system |
| CN106601917A (en) * | 2016-12-02 | 2017-04-26 | 广州光鼎科技有限公司 | Preparation method of lead-free organic and inorganic cation common hybridization perovskite material and film thereof |
| CN106757372A (en) * | 2016-11-25 | 2017-05-31 | 太原理工大学 | A kind of methylamine lead iodine perovskite monocrystalline microcavity and preparation method thereof |
| CN107779840A (en) * | 2016-08-25 | 2018-03-09 | 杭州纤纳光电科技有限公司 | The evaporation equipment and its application method of a kind of perovskite thin film and application |
| CN108321299A (en) * | 2018-02-22 | 2018-07-24 | 南京工业大学 | A kind of unleaded perovskite thin film of low-dimensional and its unleaded perovskite preparation method of solar battery |
| CN108823627A (en) * | 2018-07-18 | 2018-11-16 | 河南工业大学 | A kind of compound H-TiO of full-inorganic non-lead perovskite2The preparation of based nanotube array |
| CN108847455A (en) * | 2018-06-12 | 2018-11-20 | 北京工业大学 | A method of growth perovskite thin film |
| CN109449295A (en) * | 2018-10-30 | 2019-03-08 | 暨南大学 | Method for preparing perovskite film based on two-step printing |
| CN110071218A (en) * | 2019-04-15 | 2019-07-30 | 南京邮电大学 | A kind of method that electro-deposition prepares unleaded perovskite thin film |
| CN111233711A (en) * | 2020-01-21 | 2020-06-05 | 广东聚华印刷显示技术有限公司 | Perovskite material, preparation method thereof and light-emitting diode |
| CN111416045A (en) * | 2019-01-07 | 2020-07-14 | 南京工业大学 | Preparation method of non-lead perovskite material, material and device |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106252460A (en) * | 2016-08-15 | 2016-12-21 | 常州大学 | The manufacture method of a kind of large area perovskite solaode and system |
| CN107779840A (en) * | 2016-08-25 | 2018-03-09 | 杭州纤纳光电科技有限公司 | The evaporation equipment and its application method of a kind of perovskite thin film and application |
| CN106757372A (en) * | 2016-11-25 | 2017-05-31 | 太原理工大学 | A kind of methylamine lead iodine perovskite monocrystalline microcavity and preparation method thereof |
| CN106601917A (en) * | 2016-12-02 | 2017-04-26 | 广州光鼎科技有限公司 | Preparation method of lead-free organic and inorganic cation common hybridization perovskite material and film thereof |
| CN108321299A (en) * | 2018-02-22 | 2018-07-24 | 南京工业大学 | A kind of unleaded perovskite thin film of low-dimensional and its unleaded perovskite preparation method of solar battery |
| CN108847455A (en) * | 2018-06-12 | 2018-11-20 | 北京工业大学 | A method of growth perovskite thin film |
| CN108823627A (en) * | 2018-07-18 | 2018-11-16 | 河南工业大学 | A kind of compound H-TiO of full-inorganic non-lead perovskite2The preparation of based nanotube array |
| CN109449295A (en) * | 2018-10-30 | 2019-03-08 | 暨南大学 | Method for preparing perovskite film based on two-step printing |
| CN109449295B (en) * | 2018-10-30 | 2023-09-22 | 麦耀华 | Method for preparing perovskite film based on two-step printing |
| CN111416045A (en) * | 2019-01-07 | 2020-07-14 | 南京工业大学 | Preparation method of non-lead perovskite material, material and device |
| CN110071218A (en) * | 2019-04-15 | 2019-07-30 | 南京邮电大学 | A kind of method that electro-deposition prepares unleaded perovskite thin film |
| CN110071218B (en) * | 2019-04-15 | 2022-09-06 | 南京邮电大学 | Method for preparing lead-free perovskite film through electrodeposition |
| CN111233711A (en) * | 2020-01-21 | 2020-06-05 | 广东聚华印刷显示技术有限公司 | Perovskite material, preparation method thereof and light-emitting diode |
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Application publication date: 20160615 |