CN104134720A - Preparation method of organic and inorganic hybridization perovskite material growing by single-source flash evaporation method and plane solar cell of material - Google Patents

Preparation method of organic and inorganic hybridization perovskite material growing by single-source flash evaporation method and plane solar cell of material Download PDF

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CN104134720A
CN104134720A CN201410327199.9A CN201410327199A CN104134720A CN 104134720 A CN104134720 A CN 104134720A CN 201410327199 A CN201410327199 A CN 201410327199A CN 104134720 A CN104134720 A CN 104134720A
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inorganic hybridization
hybridization perovskite
organic inorganic
evaporation
solar cell
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徐闰
袁野
徐海涛
王文贞
葛升
徐飞
王林军
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University of Shanghai for Science and Technology
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/0001Processes specially adapted for the manufacture or treatment of devices or of parts thereof
    • H01L51/0002Deposition of organic semiconductor materials on a substrate
    • H01L51/0008Deposition of organic semiconductor materials on a substrate using physical deposition, e.g. sublimation, sputtering
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/0032Selection of organic semiconducting materials, e.g. organic light sensitive or organic light emitting materials
    • H01L51/0077Coordination compounds, e.g. porphyrin
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/42Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for sensing infra-red radiation, light, electro-magnetic radiation of shorter wavelength or corpuscular radiation and adapted for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation using organic materials as the active part, or using a combination of organic materials with other material as the active part; Multistep processes for their manufacture
    • H01L51/4213Comprising organic semiconductor-inorganic semiconductor hetero-junctions
    • H01L51/422Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2
    • H01L51/4226Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2 the wideband gap semiconductor comprising titanium oxide, e.g. TiO2
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES; ELECTRIC SOLID STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H01L51/00Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof
    • H01L51/42Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for sensing infra-red radiation, light, electro-magnetic radiation of shorter wavelength or corpuscular radiation and adapted for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation using organic materials as the active part, or using a combination of organic materials with other material as the active part; Multistep processes for their manufacture
    • H01L51/4213Comprising organic semiconductor-inorganic semiconductor hetero-junctions
    • H01L51/422Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2
    • H01L51/4233Majority carrier devices using sensitisation of widebandgap semiconductors, e.g. TiO2 the wideband gap semiconductor comprising zinc oxide, e.g. ZnO
    • 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
    • Y02E10/549Organic PV cells
    • 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

The invention relates to a preparation method of an organic and inorganic hybridization perovskite material growing by a single-source flash evaporation method and a plane solar cell of the material, and belongs to the field of novel material device manufacturing technologies. A preparation method of an organic and inorganic hybridization perovskite film comprises the step of rapidly heating a metal evaporation boat to be above 1000 DEG C by taking a perovskite material solution as a single evaporation source within 1s to prepare the organic and inorganic hybridization perovskite film with accurate components. The organic and inorganic hybridization perovskite film prepared by the single-source flash evaporation method has the characteristics that the film is high in evaporation rate and cavity-free, and is suitable for preparing a plane device. TiO2 or ZnO serving as an n-type material, Spiro-OMeTAD serving as a p-type material and the i-type organic and inorganic hybridization perovskite film form a p-i-n-type plane solar cell device; and the device with efficiency of 6.26% can be obtained after preparation condition optimization.

Description

The preparation method of single source flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof
Technical field
The preparation method who the present invention relates to a kind of single source flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, belongs to new material device fabrication field.
Background technology
The world today, along with day by day reducing and the continuous increase of the mankind to energy demand of earth resource, energy crisis is extremely urgent.For survival and development, the mankind must seek to substitute the reproducible clean new forms of energy of conventional energy resource, and one of selection is wherein solar power generation.Solar energy has and stores hugely, never exhausted, cleanliness without any pollution, is not subject to the advantages such as regional limits, is the most important new forms of energy of the mankind.
At present solar cell mainly comprises crystal silicon cell and thin-film solar cells, and wherein thin-film solar cells is few because producing materials, low price, and the advantage such as plasticity is good becomes the development trend of solar-energy photo-voltaic cell.Now, the hull cell material of two kinds of main flow industrialization is cadmium telluride (CdTe) and Copper Indium Gallium Selenide (CIGS), and they all contain element rare in the earth's crust (Te and In), are therefore not suitable for large-scale production.Recently, a kind of with CH 3nH 3pbI 3for the organic inorganic hybridization perovskite material thin-film solar cells of representative has obtained the extensive concern of academia.The contained element of this class organic inorganic hybridization perovskite material is in the earth's crust is rich in element, can be mass-produced, and cheap.From 2012, with CH 3nH 3pbI 3in research for absorbent body layer solar cell, its conversion efficiency rose violently rapidly in short 1 year, had broken through 15%.By in June, 2014, the peak efficiency of empirical tests can reach 17.9%.This makes this material very likely become follow-on main flow thin-film solar cells material, thereby has also attracted large quantities of researchers' both domestic and external concern.The preparation method of this material is mainly chemical method.As spin-coating method and the two-step method based on spin-coating method etc.These two kinds of methods all can be based on porous material TiO 2with in ZnO, deposit high-quality film, thereby obtain high efficiency.But not too applicable for planar device, chief reason is that this material material in the time that after-bake is annealed is easy to cohesion and forms large crystal grain, thereby makes large intergranule occur cavity.This will reduce the absorption of photon, and reduces parallel resistance simultaneously, and device efficiency is reduced.On the other side, the method based on vacuum can obviously be improved film coverage.As adopting double source method, Henry Snaith can prepare the film without empty little crystal grain, but double source method control complexity, two being operated in the speed of determining ratio that independently evaporation source need to be stable.In addition, for realizing high-quality thin film, very slow of evaporation rate, generally need to be controlled at 0.5 dust per second in.Low like this speed is not suitable for large-scale production.
Summary of the invention
For the defect of prior art existence, the object of this invention is to provide the preparation method of a kind of single source flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof.Adopt solution or the powder of organic inorganic hybridization perovskite material to do evaporation source, directly prepare the absorbed layer of perovskite thin film as solar cell with single source flash method, and prepare corresponding solar cell device, for the organic inorganic hybridization perovskite thin film solar cell of preparing high conversion efficiency provides a kind of new technique.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for single source flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, has following technical process and step:
A, transparent conducting glass is carried out to preliminary treatment;
B, on transparent conducting glass, deposit N-shaped TiO 2or ZnO, then put on the sample stage of vacuum evaporation apparatus as substrate;
C, organic inorganic hybridization perovskite material is dissolved in organic solvent, is prepared into organic inorganic hybridization perovskite solution or powder;
D, evaporation of metal boat is carried out to preliminary treatment;
E, organic inorganic hybridization perovskite solution or powder are laid on evaporation of metal boat uniformly;
F, at vaporization chamber air pressure lower than 5 × 10 -3under the condition of the vacuum of Pa or inert gas or nitrogen atmosphere, by flash method by organic inorganic hybridization perovskite evaporation to substrate, form film;
G, the film that evaporation is completed carry out post annealed processing;
H, on the organic inorganic hybridization perovskite thin film material preparing spin coating hole transmission layer;
I, electrode evaporation, obtain plane organic inorganic hybridization perovskite solar cell.
In described step a, transparent conducting glass is FTO, mixes the SnO of F 2; Or AZO, mix the ZnO of Al; Or ITO, mix the In of Sn 2o 3; Pre-treatment step is: first adopt Qu Latong to clean glass surface, then with deionized water, the remaining Qu Latong in surface is rinsed out, adopt afterwards acetone ultrasonic cleaning 15 minutes, then use deionized water rinsing surface, use again afterwards ethanol ultrasonic cleaning 15 minutes, use again deionized water rinsing surface, subsequently by its oven dry; Finally adopt UV ozone or Microwave plasma treatment surface.
In described step b, on transparent conducting glass, deposit N-shaped TiO 2or ZnO, deposition process can adopt magnetron sputtering method, spin coating or spray-on process.The TiO of gained 2to use as substrate with ZnO, deposit organic inorganic hybridization perovskite material thereon.
In described step c, organic inorganic hybridization perovskite solution or powder refer to and comprise CH 3nH 3pbX 3and CH 3nH 3snX 3at interior ABX 3solution or the powder of type organic inorganic hybridization perovskite material, wherein A refers to similar CH 3nH 3positive monovalence organic molecule group, B is the divalent metal element of making a comment or criticism, X refers to negative monovalence halogen.
In described steps d, evaporation of metal boat refers to tantalum piece or molybdenum sheet or tungsten sheet.Metal boat is carried out to preliminary treatment, refers to and first adopt acetone, ethanol and deionized water to clean successively to metal surface, after drying up with UV ozone or plasma treatment metal surface.
In described step f, refer to vaporization chamber air pressure is evacuated to lower than 5 × 10 by flash method evaporation organic inorganic hybridization perovskite thin film -3pa, continue to keep pumping speed to keep this vacuum degree, or close vacuum pump or valve, or pass into inert gas or nitrogen to 1-100Pa, then load 80-250A electric current, organic inorganic hybridization perovskite solution or powder are rapidly heated to 1000-1500 DEG C within the time that is less than 1 second, and whole evaporation process is less than 5 seconds.Substrate adopts the TiO of indication in step b 2or ZnO, substrate can remain on room temperature condition, also can remain on the temperature of 100-150 DEG C.
The film in described step g, evaporation being completed carries out post annealed processing and refers to that organic inorganic hybridization perovskite thin film that evaporation is completed toasts 5-40 minute under the condition of nitrogen atmosphere and 90-150 DEG C, forms film fine and close, well-crystallized.
In described step h, on the organic inorganic hybridization perovskite thin film material preparing, spin coating hole transmission layer refers to Spiro-OMeTAD or P3HT is spin-coated on as hole transmission layer on the perovskite thin film material that evaporation completes.
Electrode evaporation in described step I, obtain plane organic inorganic hybridization perovskite solar cell and refer to the material surface after spin coating hole transmission layer, by gold or the silver electrode of the method evaporation definite shape of vacuum evaporation, thereby obtain plane organic inorganic hybridization perovskite solar cell.
The present invention compared with the existing technology, has following remarkable advantage:
The present invention proposes the high physical growth method of a kind of growth rate simple to operate, and single source flash method is prepared organic inorganic hybridization perovskite thin film material, and has obtained high efficiency solar cell device, and process is simple, easy operating, favorable repeatability.This preparation method uses the solution of perovskite material to do evaporation source, makes it on metal boat, form smooth thin layer in the time vacuumizing, and the film surface of preparing is without cavity and even.Single source of the present invention flash method belongs to high speed evaporation, is easy to large-scale production.By the method, finally can implementation efficiency the preparation of the perovskite solar cell that is 6.26%.
Brief description of the drawings
Fig. 1 is CH prepared by single source flash method 3nH 3pbI 3film X-ray diffractogram.
Fig. 2 is CH prepared by single source flash method 3nH 3pbI 3the scanning electron microscope diagram of film.
Fig. 3 is CH prepared by single source flash method 3nH 3pbI 3the current/voltage figure of thin-film solar cells, test is under the illumination condition of 1.5AM.
Embodiment
Below in conjunction with accompanying drawing, specific embodiments of the invention are further described.
embodiment 1
A preparation method for single source flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, has following technical process and step:
(1) by transparent conducting glass SnO 2: F is as deposition substrate, first adopt Qu Latong clean surface, then with clear water, the remaining Qu Latong in surface is rinsed out, adopt afterwards acetone ultrasonic cleaning 15 minutes, then use deionized water rinsing surface, use again afterwards ethanol ultrasonic cleaning 15 minutes, then use deionized water rinsing surface, subsequently by its oven dry.Finally adopt UV ozone to process 10 minutes.
(2) at pretreated transparent conducting glass SnO 2: F is upper, adopts the method depositing Ti O of magnetron sputtering 2, this process adopts high-purity Ti O 2as sputtering target material, first sputtering chamber is evacuated to 5 × 10 -3pa, then passes into Ar gas, and sputtering pressure remains on 0.6Pa, and sputtering power is 150W, and sputtering time 36 minutes can be at transparent conducting glass SnO 2: the fine and close TiO of the upper deposition of F one deck 50 nanometer thickness 2film.
(3) the N-shaped TiO of 50 nanometers will be scribbled 2transparent conducting glass SnO 2: F puts on the sample stage of vacuum evaporation apparatus.Subsequently CH 3nH 3i and PbI 2powder be dissolved in ethanol according to the ratio of 1.5:1, thereby be mixed with CH 3nH 3pbI 3solution, wherein the mass percent of solution is 40%.
(4) CH 3nH 3pbI 3solution is applied on molybdenum sheet uniformly.At cavity air pressure lower than 5 × 10 -3under the condition that Pa and sample substrate temperature are room temperature, by flash method evaporation perovskite thin film.Perovskite material is rapidly heated to 1000 DEG C within the time of 1 second, and electric current used is 200 amperes, and whole evaporation time is 5 seconds.The thickness of film depends primarily on the distance between consumption and source and the substrate of solution.The amount of solution that the film of general 500nm needs is 100 microlitres, and the distance between source and substrate is about 12cm.Can realize the high speed deposition without empty perovskite thin film material by the method.The structure of film and surface topography are respectively as Fig. 1 and Fig. 2.
(5) on the perovskite thin film material completing at evaporation after spin coating hole transmission layer Spiro-OMeTAD, then evaporation is of a size of the silver electrode of 0.5*1cm, completes the preparation of perovskite solar cell.
By the prepared organic inorganic hybridization plane of above method solar cell, under the illumination condition of 1.5AM, this device short circuit current can reach 15.7 mA/cm 2, open circuit voltage is 820 mV, and fill factor, curve factor is 0.49, and the energy efficiency of this thin-film solar cells is 6.26%, as shown in Figure 3.Be 3.50% without the device efficiency of hole transmission layer.
embodiment 2
In full accord in the present embodiment step (1), (2), (3) and embodiment 1, difference is,
(4) CH 3nH 3pbI 3solution is applied on molybdenum sheet uniformly.At vaporization chamber air pressure lower than 5 × 10 -3after Pa, be filled with nitrogen, make vaporization chamber air pressure remain on 0.6Pa.Under the condition that is room temperature in sample substrate temperature, by flash method evaporation perovskite thin film.Perovskite material is rapidly heated to 1000 DEG C within the time of 1 second, and electric current used is 230 amperes, and whole evaporation time is 5 seconds.
(5) on the perovskite thin film material completing at evaporation after spin coating hole transmission layer Spiro-OMeTAD, then evaporation is of a size of the silver electrode of 2*2cm, completes the preparation of perovskite solar cell.
After passing into nitrogen in step (4), can obtain the more organic inorganic hybridization perovskite thin film of Large-Area-Uniform.In step (5) by the more large-area silver electrode of deposition can obtain with example 1 in approaching solar battery efficiency, be about 6% left and right.

Claims (9)

1. a preparation method for single source flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, is characterized in that having following technical process and step:
A, transparent conducting glass is carried out to preliminary treatment;
B, on transparent conducting glass, deposit N-shaped TiO 2or ZnO, then put on the sample stage of vacuum evaporation apparatus as substrate;
C, organic inorganic hybridization perovskite material is dissolved in organic solvent, is prepared into organic inorganic hybridization perovskite solution or powder;
D, evaporation of metal boat is carried out to preliminary treatment;
E, organic inorganic hybridization perovskite solution or powder are laid on evaporation of metal boat uniformly;
F, at vaporization chamber air pressure lower than 5 × 10 -3under the condition of the vacuum of Pa or inert gas or nitrogen atmosphere, by flash method by organic inorganic hybridization perovskite evaporation to substrate, form film;
G, the film that evaporation is completed carry out post annealed processing;
H, on the organic inorganic hybridization perovskite thin film material preparing spin coating hole transmission layer;
I, electrode evaporation, obtain plane organic inorganic hybridization perovskite solar cell.
2. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, is characterized in that, in described step a, transparent conducting glass is FTO, mixes the SnO of F 2; Or AZO, mix the ZnO of Al; Or ITO, mix the In of Sn 2o 3; Pre-treatment step is: first adopt Qu Latong to clean glass surface, then with deionized water, the remaining Qu Latong in surface is rinsed out, adopt afterwards acetone ultrasonic cleaning 15 minutes, then use deionized water rinsing surface, use again afterwards ethanol ultrasonic cleaning 15 minutes, use again deionized water rinsing surface, subsequently by its oven dry; Finally adopt UV ozone or Microwave plasma treatment surface.
3. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, is characterized in that, deposits N-shaped TiO in described step b on transparent conducting glass 2or ZnO, deposition process adopts magnetron sputtering method, spin coating or spray-on process; The TiO of gained 2to use as substrate with ZnO, deposit organic inorganic hybridization perovskite material thereon.
4. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, is characterized in that, in described step c, organic inorganic hybridization perovskite solution or powder refer to and comprise CH 3nH 3pbX 3and CH 3nH 3snX 3at interior ABX 3solution or the powder of type organic inorganic hybridization perovskite material, wherein A refers to similar CH 3nH 3positive monovalence organic molecule group, B is the divalent metal element of making a comment or criticism, X refers to negative monovalence halogen.
5. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, is characterized in that, in described steps d, evaporation of metal boat refers to tantalum piece or molybdenum sheet or tungsten sheet; Evaporation of metal boat is carried out to preliminary treatment, refer to and first adopt acetone, ethanol and deionized water to clean successively to metal surface, dry up rear with UV ozone or plasma treatment metal surface.
6. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, it is characterized in that, in described step f, refer to vaporization chamber air pressure is evacuated to lower than 5 × 10 by flash method evaporation organic inorganic hybridization perovskite thin film -3pa, continue to keep pumping speed to keep this vacuum degree, or close vacuum pump or valve, or pass into inert gas or nitrogen to 1-100Pa, then load 80-250A electric current, organic inorganic hybridization perovskite solution or powder are rapidly heated to 1000-1500 DEG C within the time that is less than 1 second, and whole evaporation process is less than 5 seconds.
7. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, it is characterized in that, the film in described step g, evaporation being completed carries out post annealed processing and refers to that organic inorganic hybridization perovskite thin film that evaporation is completed toasts 5-40 minute under the condition of nitrogen atmosphere and 90-150 DEG C, forms film fine and close, well-crystallized.
8. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, it is characterized in that, in described step h, on the organic inorganic hybridization perovskite thin film material preparing, spin coating hole transmission layer refers to Spiro-OMeTAD or P3HT is spin-coated on as hole transmission layer on the perovskite thin film material that evaporation completes.
9. the preparation method of single source according to claim 1 flash method growth organic inorganic hybridization perovskite material and plane solar cell thereof, it is characterized in that, electrode evaporation in described step I, obtain plane organic inorganic hybridization perovskite solar cell and refer to the material surface after spin coating hole transmission layer, by gold or the silver electrode of the method evaporation definite shape of vacuum evaporation, thereby obtain plane organic inorganic hybridization perovskite solar cell.
CN201410327199.9A 2014-07-10 2014-07-10 Preparation method of organic and inorganic hybridization perovskite material growing by single-source flash evaporation method and plane solar cell of material Pending CN104134720A (en)

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CN104916785A (en) * 2015-06-09 2015-09-16 绍兴文理学院 CH3NH3PbI3 thin-film solar cell preparation method
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Application publication date: 20141105