CN109659394A - A kind of preparation method and application of high quality full-inorganic perovskite thin film material - Google Patents

A kind of preparation method and application of high quality full-inorganic perovskite thin film material Download PDF

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CN109659394A
CN109659394A CN201811534810.XA CN201811534810A CN109659394A CN 109659394 A CN109659394 A CN 109659394A CN 201811534810 A CN201811534810 A CN 201811534810A CN 109659394 A CN109659394 A CN 109659394A
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thin film
inorganic perovskite
full
scn
perovskite thin
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陶霞
叶芝莉
郑言贞
周军帅
侯杰
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/18Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
    • H01L31/1876Particular processes or apparatus for batch treatment of the devices
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/02Details
    • H01L31/0216Coatings
    • H01L31/02161Coatings for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/02167Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005Processes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/26Materials of the light emitting region
    • 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
    • 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

A kind of preparation method and application of high quality full-inorganic perovskite thin film material, belongs to organic/inorganic composite material and optoelectronic materials technology.Mainly comprise the following steps addition Pb (SCN) in full-inorganic perovskite precursor liquid2For additive, Pb (SCN) is prepared using a step spin-coating method2The full-inorganic perovskite thin film of induction passes through Pb (SCN)2The modified full-inorganic perovskite thin film for obtaining smooth dense non-porous hole while the defects of passivation film state.Full-inorganic perovskite by using mixed halogen ion is main system, and with the growth of additive regulation perovskite thin film, additive is passivated perovskite crystal boundary, reduces film internal flaw, improves the carrier transport service life.The short-circuit current density and fill factor that battery can be significantly improved applied to photovoltaic cell using the full-inorganic perovskite thin film of this method preparation as absorbed layer, improve the photoelectric conversion efficiency and stability of full-inorganic perovskite battery.

Description

A kind of preparation method and application of high quality full-inorganic perovskite thin film material
Technical field
The invention belongs to perovskite solar battery and related photoelectric semiconductor material fields, and in particular to mixed halogen The CsPbX of ion3It is main system completely without type perovskite, is added Pb (SCN)2For additive perovskite thin film technology of preparing and Its application as absorbed layer in thin-film solar cells.
Background technique
Global energy shortage, environmental pollution, climate warming annoying human society with just getting worse." seek green Color alternative energy source realizes sustainable development " have become the common issue that countries in the world face.Solar energy is with the unlimited of its reserves Property, existing generality, the advantages such as spatter property of development and utilization become ideal alternative energy source.Currently, as clean energy resource generation The silicon solar cell of table has been carried out extensive industrialization, but the production of the silicon raw material of its industrial chain upstream be high energy consumption and High pollutive industries.For this purpose, scientist, which sets about developing, prepares " zero-emission " green solar battery with more new materials, wherein new Type nano structural material and organic/nanostructure semiconductor composite become photovoltaic energy conversion field most noticeable one A research direction.Thin-film solar cells of new generation based on the building of these material systems includes organic solar batteries (abbreviation OSC), dye-sensitized solar cells (abbreviation DSC) and perovskite solar battery (abbreviation PSC) just inner product pole in the world In research and development.Perovskite solar cell is from dye-sensitized cell evolution.Perovskite solar cell also has at low cost, preparation Simple process, and the series of advantages such as flexible, transparent and laminated cell can be prepared, so its application is more diversified.Calcium titanium The structure of pit wood material is ABX3, wherein A=CH3NH3 +(MA);CH3(NH2)2 +(FA);Cs+, B=Pb2 +;Sn2 +;Ge2 +, X=Cl-; Br-;I-Organic-inorganic perovskite is mixed as very promising next-generation photovoltaic material, by its brilliant low exciton knot Energy is closed, inorganic perovskite attracts attention as bipolar charge distribution transmission characteristic and bipolarity charge transmission.Based on perovskite Solar battery (PSC) shows up to 23.2% power conversion efficiency (PCE), although quickly growing, mixes perovskite The intrinsic volatility of middle organic component is still the key constraints survived in severe operating environments.Although having developed sun Ion exchange and encapsulation under some stress conditions to generate more stable perovskite device, but there are still overcome and all environment The challenge of the relevant degradation of parameter, including moisture corrosion, the degradation of electric field induction, heat ageing, ultraviolet light irradiation and photooxidation.Most Closely, full-inorganic caesium lead halide [CsPbX3(X=halide)] perovskite because of it to the intrinsic stability of above-mentioned stress condition and Its attractive photoelectric properties and be developed.Although perovskite CsPbBr3With extraordinary stability, but its band gap Up to 2.3eV can not absorb the light more than 540nm greatly very much.And CsPbI3Band gap with more suitable 1.73eV, but it There is extremely strong phase instability.For those reasons, double halogen perovskites are developed.Special CsPbI2Br perovskite, Its reasonable band gap is 1.91eV, is very suitable in laminated cell structure, while stability also greatly improves.
Regrettably, the polycrystalline property of the perovskite thin film of mixed halogen will generate a large amount of trap site, including be originated from The deep trap of point defect and it is present in perovskite crystal surface or the nonstoichiometric composition of grain boundaries is dominant inside photoactive layer The trap site of gesture.These may act as charge recombination center to cause serious energy loss, thus the device efficiency limited. In order to improve the short circuit current of full-inorganic perovskite battery, there is document report to prepare using solvent dimethyl sulfoxide (DMSO) higher The precursor solution of concentration can generate a large amount of holes and crystal boundary to increase full-inorganic perovskite thin film thickness simultaneously.It is worth note Meaning: crystal boundary and hole in perovskite film can cause charge recombination, and crystal grain under its relevant charge trap state Boundary can cause shallow state near valence band edge, hinder hole diffusion.Therefore, it is necessary to develop the high quality of low-density charge trap Full-inorganic perovskite thin film.For this purpose, additive is added in full-inorganic perovskite material to improve film quality is also One hot spot of current research.Therefore it provides a kind of technology of preparing of simple, low cost inorganic perovskite thin film, and be allowed to Efficiently and stably had a very important significance for perovskite battery.
Summary of the invention
In order to solve the deficiencies in the prior art, an object of the present invention is to provide a kind of inorganic perovskite thin film of high quality And preparation method thereof.
The second object of the present invention is to provide a kind of solar battery, the solar battery includes that above-mentioned high quality is complete The absorbed layer that inorganic perovskite thin film is constituted.
Inventor is the study found that using the Pb (SCN)2It is added in perovskite precursor solution, adopts as additive The few full-inorganic perovskite thin film of fine and close smooth defect can be prepared with the method, can be used for efficient perovskite thin film The absorbed layer of solar battery, and gained cell photoelectric transfer efficiency is higher, can be applied in the sub- battery of laminated cell.This The preparation method of invention is easy to operate, at low cost, and energy consumption is small, is suitble to the large-scale industrial production application of solar battery.
The present invention is achieved through the following technical solutions:
A kind of preparation method of high quality full-inorganic perovskite thin film material, which comprises the following steps:
(1)Pb(SCN)2The configuration of solution:
Pb(SCN)2The configuration method of solution are as follows: by Pb (SCN)2Powder is dissolved in dimethyl sulfoxide (DMSO), stirring at normal temperature It makes it completely dissolved, is made into Pb (SCN)2Solution, it is spare;
(2) configuration of perovskite precursor solution:
The configuration method of full-inorganic perovskite precursor solution are as follows: by one or more of inorganic halogen compounds CsX, Metal halogen compound PbX2One or more of be mixed into organic solvent, stirring at normal temperature is overnight, obtains the Huang of clear Color solution.By 1) gained Pb (SCN)2Solution is added into above-mentioned solution, and heating stirring is uniform, obtains Pb (SCN)2Addition Full-inorganic perovskite precursor solution;
(3) preparation of perovskite thin film:
In glove box, by (2) resulting addition Pb (SCN)2Full-inorganic perovskite precursor solution, pass through a step revolve The method of coating film forming, in conductive substrates or is coated in the conductive substrates of carrier transport thin layer, prepares Pb (SCN)2Addition Perovskite thin film;Then the perovskite thin film prepared is annealed, is cooled to room temperature, high quality full-inorganic perovskite is obtained Film.
X in the CsX is a kind of in I, Br, Cl.
The PbX2In X be a kind of in I, Br, Cl.
Described CsX, PbX2Molar ratio be 1:1, CsX and PbX2Molar concentration in perovskite precursor solution is preferred It is 0.6~1.2mol/l.
Organic solvent described in step (2) is one in N,N-dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) Kind or two kinds.
The Pb (SCN)2Additive amount and perovskite solution in PbX2Molar ratio be (0.5-20): 100.
40-80 DEG C of heating temperature described in step (2), the heating stirring time is 1~10h.
The method of (3) one step spin-coating method of step film forming, preferably one step spin-coating film method of anti-solvent, anti-solvent are added dropwise method and are 15~20s starts at the uniform velocity to be added dropwise after starting spin coating, and anti-solvent is added dropwise in spin coating perovskite precursor solution.Anti-solvent is added dropwise Measure every 4cm2300~400 μ l are added dropwise in area, and dropwise addition is lasted for 1~4s.Anti-solvent is chlorobenzene, in toluene, ethyl acetate, ether One or more.
The conductive substrates are FTO electro-conductive glass, ITO electro-conductive glass or flexible conducting substrate.
The material of the carrier transport thin layer is ZnO, TiO2、SnO2、C60、NiOx, any one in PCBM partly lead Body material.
Annealing described in step (3) is 200~300 DEG C of 1~30min of heating.
High quality full-inorganic perovskite thin film material the answering in the structures such as solar battery, light emitting diode With.Preferably, it is used to prepare the absorbed layer of perovskite thin film solar battery.By the other one layer of current-carrying of the film spin coating prepared Son transmission, vacuum evaporation Ag electrode are prepared into perovskite solar battery.
Compared with prior art compared with, the invention has the following advantages:
(1) of the present invention to be based on Pb (SCN)2Precursor solution for the full-inorganic perovskite of additive is at low cost It is honest and clean, easy to operate, repeatability is high;
(2) of the present invention to be based on Pb (SCN)2For the full-inorganic perovskite of additive precursor solution, pass through one Walk the full-inorganic perovskite thin film material surface densification of spin coating anti-solvent method preparation and without hole, this Pb (SCN)2In perovskite Crystal boundary passivation does not have been reported that also in the literature.Experiment show by the film preparation perovskite solar battery have compared with High photoelectric conversion efficiency.
Detailed description of the invention
The stereoscan photograph of full-inorganic perovskite thin film material prepared by Fig. 1, embodiment 1.
The atomic force microscopy of full-inorganic perovskite thin film material prepared by Fig. 2, embodiment 1.
The I-V curve of the solar battery of full-inorganic perovskite thin film material preparation prepared by Fig. 3, embodiment 1.
Specific embodiment
Below in conjunction with attached drawing and example, the invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
1)Pb(SCN)2The configuration of solution:
By Pb (SCN)2Powder is dissolved in dimethyl sulfoxide (DMSO), is stirred 1h, is made into 1mmol/ml Pb (SCN)2Solution, This solution is used as stock solution.
2) configuration of perovskite precursor solution:
Cesium bromide and lead iodide are added in pure DMSO with molar ratio 1:1, stir 1h, being configured to molar content is 0.8 Perovskite solution.Stirring at normal temperature is stayed overnight, and the yellow perovskite precursor solution of clear is obtained;Take the 1 of 10ul) gained Pb (SCN)2DMSO solution be added in above-mentioned solution, heating stirring 1h obtains Pb (SCN)2The full-inorganic perovskite forerunner of addition Liquid solution.
3) preparation of perovskite thin film:
In glove box, by the obtained Pb of step 2) (SCN)2The full-inorganic perovskite precursor solution of addition, is applying There is SnO2Conductive substrates on, using a step spin-coating method, the revolving speed of spin-coating method is 3000rpm, spin-coating time 30s, 15s drop Add 350 μ l of anti-solvent, carry out the preparation of perovskite thin film, then moves back the perovskite thin film prepared for 300 DEG C on hot plate Fiery 20min, is cooled to room temperature, and obtains high quality full-inorganic perovskite thin film.
4) application in the structures such as solar battery, light emitting diode:
High quality full-inorganic perovskite thin film is used to prepare the absorbed layer of perovskite thin film solar battery and will prepare High quality full-inorganic perovskite thin film spin coating hole transmission layer is deposited Ag electrode, is prepared into perovskite solar battery.
As can be seen that being based on Pb (SCN) from Fig. 1 and Fig. 22As the perovskite thin film material of additive preparation, film Surface compact and without hole, particle is uniform and has lower roughness.
From figure 3, it can be seen that being based on Pb (SCN)2Perovskite made of perovskite thin film material as additive preparation Solar battery, in standard sources (AM1.5G, 100mW/cm2) irradiation under, measure the i-v curve of battery, calculate The photoelectric conversion efficiency of perovskite solar energy.As can be seen that this be added to Pb (SCN)2The perovskite thin film material of additive Manufactured full-inorganic perovskite solar battery, photoelectric conversion efficiency with higher, photoelectric conversion efficiency 12.17%.
Embodiment 2
1)Pb(SCN)2The configuration of solution:
By Pb (SCN)2Powder is dissolved in dimethyl sulfoxide (DMSO), is stirred 1h, is made into 1mmol/ml Pb (SCN)2Solution, This solution is used as stock solution.
2) configuration of perovskite precursor solution:
Cesium bromide and lead iodide are added in pure DMSO with molar ratio 1:1, stir 1h, being configured to molar content is 1.0 Perovskite solution.Stirring at normal temperature is stayed overnight, and the yellow perovskite precursor solution of clear is obtained;Take the 1 of 20ul) gained Pb (SCN)2DMSO solution be added in above-mentioned solution, heating stirring 1h obtains Pb (SCN)2The full-inorganic perovskite forerunner of addition Liquid solution.
3) preparation of perovskite thin film:
In glove box, by the obtained perovskite precursor solution of step 2), it is being coated with SnO2Conductive substrates on, adopt With a step spin-coating method, the revolving speed of spin-coating method is 3000rpm, and spin-coating time 30s, 15s are added dropwise 350 μ l of anti-solvent, carry out calcium The preparation of titanium ore film will then prepare perovskite thin film 300 DEG C of annealing 20min on hot plate, and be cooled to room temperature, obtain height Quality full-inorganic perovskite thin film.
4) application in the structures such as solar battery, light emitting diode:
High quality full-inorganic perovskite thin film is used to prepare the absorbed layer of perovskite thin film solar battery and will prepare High quality full-inorganic perovskite thin film spin coating hole transmission layer is deposited Ag electrode, is prepared into perovskite solar battery.

Claims (10)

1. a kind of preparation method of high quality full-inorganic perovskite thin film material, which comprises the following steps:
(1)Pb(SCN)2The configuration of solution:
Pb(SCN)2The configuration method of solution are as follows: by Pb (SCN)2Powder is dissolved in dimethyl sulfoxide (DMSO), and stirring at normal temperature makes it It is completely dissolved, is made into Pb (SCN)2Solution, it is spare;
(2) configuration of perovskite precursor solution:
The configuration method of full-inorganic perovskite precursor solution are as follows: by one or more of inorganic halogen compounds CsX, metal Halogen compounds PbX2One or more of be mixed into organic solvent, stirring at normal temperature is overnight, and the yellow for obtaining clear is molten Liquid.By 1) gained Pb (SCN)2Solution is added into above-mentioned solution, and heating stirring is uniform, obtains Pb (SCN)2Addition completely without Machine perovskite precursor solution;
(3) preparation of perovskite thin film:
In glove box, by (2) resulting addition Pb (SCN)2Full-inorganic perovskite precursor solution, pass through a step spin-coating method The method of film forming in conductive substrates or is coated in the conductive substrates of carrier transport thin layer, is prepared Pb (SCN)2The calcium titanium of addition Mine film;Then the perovskite thin film prepared is annealed, is cooled to room temperature, it is thin to obtain high quality full-inorganic perovskite Film.
2. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that X in the CsX is a kind of in I, Br, Cl.
3. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that The PbX2In X be a kind of in I, Br, Cl.
4. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that Described CsX, PbX2Molar ratio be 1:1, CsX and PbX2Molar concentration in perovskite precursor solution is 0.6~ 1.2mol/l。
5. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that Organic solvent described in step (2) is one or both of N,N-dimethylformamide (DMF) and dimethyl sulfoxide (DMSO).
The Pb (SCN)2Additive amount and perovskite solution in PbX2Molar ratio be (0.5-20): 100.
6. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that 40-80 DEG C of heating temperature described in step (2), the heating stirring time is 1~10h.
7. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that The method of (3) one step spin-coating method of step film forming is one step spin-coating film method of anti-solvent, and it is after starting spin coating that method, which is added dropwise, in anti-solvent 15~20s is at the uniform velocity added dropwise, and anti-solvent is added dropwise in spin coating perovskite precursor solution;The every 4cm of anti-solvent dripping quantity2Area drop Add 300~400 μ l, dropwise addition is lasted for 1~4s;Anti-solvent is one or more of chlorobenzene, toluene, ethyl acetate, ether.
8. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that The conductive substrates are FTO electro-conductive glass, ITO electro-conductive glass or flexible conducting substrate;The carrier transport thin layer Material is ZnO, TiO2、SnO2、C60、NiOx, any one semiconductor material in PCBM.
9. a kind of preparation method of high quality full-inorganic perovskite thin film material described in accordance with the claim 1, which is characterized in that Annealing described in step (3) is 200~300 DEG C of 1~30min of heating.
10. the high quality full-inorganic perovskite thin film material that any one of claim 1-9 the method is prepared must be applied, Application in solar battery, light emitting diode construction;Preferably, it is used to prepare the absorption of perovskite thin film solar battery Layer.
CN201811534810.XA 2018-12-14 2018-12-14 A kind of preparation method and application of high quality full-inorganic perovskite thin film material Pending CN109659394A (en)

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CN110289332A (en) * 2019-07-02 2019-09-27 中国建材国际工程集团有限公司 A kind of preparation method and structure of laminated cell
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CN111403607A (en) * 2020-03-25 2020-07-10 华东理工大学 Chelated perovskite material, film, device and preparation method and application thereof
CN114808124A (en) * 2022-03-16 2022-07-29 暨南大学 Preparation method of mixed halide perovskite single crystal and polycrystalline film
CN114808124B (en) * 2022-03-16 2023-01-03 暨南大学 Preparation method of mixed halide perovskite single crystal and polycrystalline film
CN115108733A (en) * 2022-07-04 2022-09-27 桂林电子科技大学 Method for patterning all-inorganic perovskite microcrystal composite film

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