CN102856499A - Preparation method for SnO2 and P3HT hybridization heterojunction thin-film solar cell - Google Patents
Preparation method for SnO2 and P3HT hybridization heterojunction thin-film solar cell Download PDFInfo
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- CN102856499A CN102856499A CN2012102927215A CN201210292721A CN102856499A CN 102856499 A CN102856499 A CN 102856499A CN 2012102927215 A CN2012102927215 A CN 2012102927215A CN 201210292721 A CN201210292721 A CN 201210292721A CN 102856499 A CN102856499 A CN 102856499A
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Abstract
The invention relates to a preparation method for a SnO2 and P3HT hybridization heterojunction thin-film solar cell. The method comprises the following steps of: conducting hydrothermal and solvotherma treatment to prepare a SnO2 thin film on an ITO conductive glass substrate by taking sulfur powder, ammonium persulfate and metal tin target as raw materials and absolute ethyl alcohol, DMF and distilled water as solvents. SnS is synthesized by using a solvothermal method, the SnS is used as a precursor for preparing the SnO2, and oxidization reaction from SnO<2+> to Sn4<+> is simpler and is low in energy consumption; the shape of the synthesized SnS has a platy connection net structure and can provide a template for the growth of the SnO2, loose structure distributed evenly is prepared, the specific surface area of the SnO2 thin film is increased, the two are better contacted when being mutually penetrated with P3HT hybridization for a net so as to improve the photoelectricity conversion property of the device. In addition, P3HT is spin-coated on the surface, annealing treatment is carried out at 120 DEG C for 2h, so that the SnO2 and P3HT hybridization heterojunction thin film is obtained. The steps of the method are simple, and no surface active agent and other chemical additive are required for use.
Description
Technical field
The invention belongs to material chemistry technical field, relate in particular to and a kind ofly in the substrate of ITO electro-conductive glass, prepare SnO
2method with the hetero-junction thin-film of P3HT hydridization.
Background technology
The global energy demand increases year by year, and the exploitation of solar energy have become the hot subject of World Focusing.In the development course of solar cell, can be divided into and take the first generation solar cell that monocrystalline silicon and polysilicon be material, utilize thin-film material to complete the second generation solar cell of opto-electronic conversion, introduce the third generation solar cell of organic substance and inorganic nano science and technology on the basis of hull cell, the 4th battery eliminator is mainly sandwich construction.People just constantly find new materials and methods, and expectation is used simple production technology to prepare the solar cell of low-cost high-efficiency.The organic thin film solar cell receives very big concern, utilizes organic solubility, at normal temperatures and pressures directly in the electrode surface film forming, forms active layer.But, because the charge mobility of organic substance self is lower, therefore its energy conversion efficiency is unsatisfactory so far.Different from organic substance, mostly inorganic semiconductor material all has higher charge mobility, so the comprehensive organic substance of people and inorganic matter advantage are separately prepared the solar cell of organic inorganic hybridization film.
The Alivisatos seminar in the vertical university's Berkeley of California, USA branch school has reported that use CdSe semiconductor nanorods is as acceptor, the conjugated polymer prepared with the P3HT blend/inorganic semiconductor nano-crystal hybrid thin film solar cell, energy efficiency reaches 1.7%.The semi-conductive polymer of n type inorganic semiconductor and p type forms interpenetrating networks, inorganic semiconductor material as electron acceptor has the following advantages: the energy level of (1) nano particle and band gap can be regulated by the kind and the size that change nano particle, make it at whole visible-range, absorption be arranged, can enlarge the absorption region of polymer organic layer to solar spectrum, improve the matching of battery response spectrum and solar radiation; (2) nano material has higher electron mobility, and chemical stability is better.On this basis, people use other inorganic semiconductor material (ZnO, ZnS, TiO
2deng) with organic substance (P3HT or MEHPPV) hydridization, prepare the solar cell device of a series of similar structures, and efficiency also brings up to 5.06%.This has opened a new field for the nanocrystalline application of inorganic semiconductor, attracts wide attention.
SnO
2belong to a kind of broad-band gap N-shaped semi-conducting material, its direct band gap is 3.6eV, as a kind of environment-friendly type semi-conducting material, the advantages such as electron-transporting is good, synthesis technique is simple, cost is low, toxicity is low owing to having, good stability, long service life, there is very high using value in the photocell field, it is applied in lithium ion battery and dye-sensitized cell mostly at present, and for SnO
2the report of doing the thin-film solar cells aspect with conjugatd polymers hydridization seldom.In addition, with regard to current similar preparation research, the preparation of this class material greatly mainly with metallic tin salt as Xi Yuan, adopt water and solvent-thermal method or sol-gel process to prepare SnO
2nano-powder material, then utilize and scrape the preparation that the skill in using a kitchen knife in cookery or spin coating technique etc. carry out film; Or plantation one deck crystal seed carries out induced growth formation film in substrate.But, at the assembling solar photovoltaic device, there are some defects in testing photoelectronic conversion performance aspect: the first, in preparation process experimental procedure require loaded down with trivial details, condition harshness, and can use some poisonous reactant or solvents, health risk, pollute; The second, in film forming procedure, the technology such as crystal seed induced growth or spin-coating method are difficult to control to thickness and the distribution consistency degree of film; Therefore, with organic polymer, carrying out compound tense, can directly affect composite effect, thereby affect photoelectric conversion efficiency.Therefore, for the semi-conducting material that significant application value is arranged, no matter commercial Application or laboratory research, all material preparation technology is had higher requirement, adopt the raw material of simple technique, cheapness, the reduce energy consumption, synthesize environmentally safe, highly purified product, to meet the preparation requirement under current shortage of resources, energy deficiency condition.
The present invention adopts water and solvent-thermal method under cryogenic conditions to realize SnO
2the preparation of nano film material, and, by itself and P3HT hydridization, the hetero-junction thin-film solar cell photovoltaic device of assembling organic inorganic hybridization, study its opto-electronic conversion performance.Whole preparation process is easy and simple to handle, environmental protection, and energy consumption is low, uses cost of material cheap, without any murder by poisoning accessory substance.
Summary of the invention
Problem to be solved by this invention is: a kind of directly synthetic SnO of water at low temperature and solvent heat in the electro-conductive glass substrate is provided
2the chemical method of nano film material, and by itself and P3HT hydridization, preparation SnO
2with P3HT(SnO
2/ P3HT) the hetero-junction thin-film solar cell device of hydridization.
the technical scheme that the present invention takes the problem that will solve is:
of the present inventiona kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid, it is ITO/SnO
2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.
of the present inventiona kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid in, SnO
2nano film material original position at low temperatures prepares, and method is with nanometer Sn
(0)for Xi Yuan, in the ITO electro-conductive glass substrate that is coated with metallic tin, by hydro-thermal and solvent heat two step wet chemicals, synthesize SnO
2nano film material, this thin-film material thickness is regulated and controled by reaction temperature and reaction time condition.
of the present inventiona kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid in, SnO
2the nano film material method that at low temperatures prepared by original position is, at first utilize magnetron sputtering sputter layer of metal tin in the substrate of ITO electro-conductive glass, by this sputter the ITO electro-conductive glass sheet inclined side of layer of metal tin be put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then add each 10mL of absolute ethyl alcohol and DMF, be placed at 160 ℃ of temperature solvent thermal reaction 4 hours, product uses distilled water and absolute ethanol washing more than 2 times, is drying to obtain the SnS film standby; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add the 3mg ammonium persulfate as oxidant, with the distillation water as solvent, the volume of distilled water is vessel volume 1/2~2/3, in temperature, be to react 24 hours at 140 ℃ of temperature, product uses distilled water and absolute ethanol washing more than 2 times, and drying at room temperature obtains SnO
2nano film material.
of the present inventiona kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid in, SnO
2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells, be, at first utilize magnetron sputtering sputter layer of metal tin in the substrate of ITO electro-conductive glass, by this sputter the ITO electro-conductive glass sheet inclined side of layer of metal tin be put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then add each 10mL of absolute ethyl alcohol and DMF, be placed at 160 ℃ of temperature solvent thermal reaction 4 hours, product uses distilled water and absolute ethanol washing more than 2 times, is drying to obtain the SnS film standby; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add the 3mg ammonium persulfate as oxidant, with the distillation water as solvent, the volume of distilled water is vessel volume 1/2-2/3, in temperature, be to react 24 hours at 140 ℃ of temperature, product uses distilled water and absolute ethanol washing more than 2 times, and drying at room temperature obtains SnO
2nano thin-film;
Then in vacuum glove box, utilize spin-coating method that the P3HT of the 10mg/mL for preparing is spun on to prepared SnO
2the nano thin-film surface, 120 ℃ of annealing in process 2 hours, obtain SnO
2with P3HT hybrid heterojunctions thin-film solar cells.
Take a certain amount of P3HT and be dissolved in chloroform the solution that is configured to 10 mg/mL, 40
oc adds thermal agitation fully dissolves it.This composite film material is to be prepared the SnO of loose structure by solvent-thermal method under low temperature
2thin-film material, the method for process spin-coating is at its surperficial spin coating one deck P3HT, and the n type inorganic semiconductor of preparation and p type semi-conducting polymer form the hetero-junction thin-film of interpenetrating networks.
of the present inventionthe preparation method of the hetero-junction thin-film solar cell device of inorganic/organic hybrid: first by step described above, prepare SnO
2put into high vacuum ion evaporation instrument with P3HT hybrid heterojunctions thin-film material, by mode evaporation one deck aluminium electrode (vacuum degree 9.0 * 10 of thermal evaporation
-5mbar), assemble to obtain ITO/SnO
2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.
in the present inventionat first utilize solvent-thermal method to synthesize SnS, it is at preparation SnO
2process in serve as predecessor, from Sn
2+to Sn
4+oxidation reaction simpler, consume energy low; In addition, synthetic SnS pattern is the network configuration that sheet connects, and can be SnO
2growth template is provided, prepare the open structure be evenly distributed, increase SnO
2the specific area of film, have better the contact while making to form network interpenetrating with P3HT hydridization, to improve the opto-electronic conversion performance of its device.
The present invention adopts cheap raw material, and the sulphur powder, ammonium persulfate, metal tin target, with absolute ethyl alcohol, DMF(N, dinethylformamide), the distillation water as solvent, can in the substrate of ITO electro-conductive glass, prepare SnO through simple hydro-thermal and solvent heat heat treatment
2film.The method step is simple, again without using any surfactant and other chemical addition agent, only need be by ammonium persulfate, synthetic predecessor film SnS adds in reactor, and hydro-thermal reaction is taken out after a few hours, water and ethanol cyclic washing, natural drying, can obtain white transparent, be evenly distributed, have the SnO of open structure
2film.Then adopt spin coating technique to be coated with the poly-3-hexyl thiophene conjugated polymer of P3HT(on its surface), 120 ℃ of annealing in process 2h, obtain SnO
2hetero-junction thin-film with P3HT hydridization.
advantage of the present invention:
1, for the present invention, distilled water, ethanol, DMF, as reaction medium, without using the solvent that toxicity is larger, belong to environmentally friendly reaction.
2, the present invention is low-temp reaction, and reaction only need add reaction raw materials in reactor, just can obtain required product under 140 ℃, does not need to use any surfactant, and the reaction raw materials cost is low, and energy consumption is low, and experimental implementation is simple simultaneously.
3, the present invention is first by SnO
2nano semiconductor material and P3HT hydridization prepare SnO
2with P3HT (SnO
2/ P3HT) hetero-junction thin-film of hydridization is applied to the assembling solar battery device.
The present invention has important Research Significance for carrying out synthesizing organic-inorganic bulk-heterojunction composite material.
The accompanying drawing explanation
The SnO of Fig. 1, embodiment 1 preparation
2the scanning electron micrograph of thin-film material
The SnO of Fig. 2, embodiment 2 preparations
2the scanning electron micrograph of thin-film material
The SnO of Fig. 3, embodiment 3 preparations
2the scanning electron micrograph of thin-film material
The SnO of Fig. 4, embodiment 3 preparations
2thin-film material X-ray diffraction pattern (XRD)
In XRD diffraction result, can find out, be ITO substrate diffraction maximum except what mark ★, and other diffraction maximums are SnO
2diffraction maximum, corresponding crystal face marks, other impurity peaks do not occur;
The SnO of Fig. 5, embodiment 3 preparations
2the hetero-junction thin-film solar cell device schematic diagram of/P3HT hydridization
In figure: 1-substrate of glass, 2-ITO, 3-SnO
2/ P3HT, 4-Al, 5-insulating barrier;
The SnO of Fig. 6, embodiment 3 preparations
2the I-V curve of the hetero-junction thin-film solar cell device of/P3HT hydridization
The open circuit voltage of this battery (Voc) is 0.405V, and density of photocurrent (Jsc) is 0.321mA/cm
2, fill factor, curve factor (FF) is 15.52%, the electricity conversion of this battery is 0.02% at present.
Embodiment
Further illustrate the present invention below by embodiment.
1, preparation: volume 30mL polytetrafluoroethylene reactor is respectively washed 1-3 time with running water, distilled water, absolute ethyl alcohol successively, dry rear stand-by; Utilize magnetron sputtering sputter in the substrate of ITO electro-conductive glass
100nmthick metal Sn is stand-by.
2, reactions steps: add 3mg sulphur powder in the clean polytetrafluoroethylene of volume 30mL, then add absolute ethyl alcohol and each 10mL of DMF, be uniformly mixed, then use the above-mentioned sputter of clean tweezers gripping
?the ITO electro-conductive glass sheet inclined side of metal Sn is put in volume 30mL polytetrafluoroethylene reactor, makes metal covering upward, and reaction is 4 hours under 160 ℃, product respectively washs 3 times with distilled water and absolute ethyl alcohol, 60 ℃ of dryings of constant temperature make the SnS film in the substrate of ITO electro-conductive glass sheet, standby; In the clean polytetrafluoroethylene reactor of volume 30mL, add the 3mg ammonium persulfate as oxidant, add distilled water 20mL, stirring and dissolving, then be put in the SnS film inclined side of preparation in its polytetrafluoroethylene reactor,
120 ℃ are reacted 18 hours, product is respectively washed 3 times with distilled water and absolute ethyl alcohol, 60 ℃ of dry SnO that obtain of constant temperature
2the film product, product is white transparent membrane.Microstructure under scanning electron microscopy is the equally distributed open structure of nano particle, and scanning electron micrograph is shown in Fig. 1.
1, preparation: volume 30mL polytetrafluoroethylene reactor is respectively washed 2 times with running water, distilled water, absolute ethyl alcohol successively, dry rear stand-by; Utilize magnetron sputtering sputter in the substrate of ITO electro-conductive glass
200nmthick metal Sn is stand-by.
2, reactions steps: add 3mg sulphur powder in the clean polytetrafluoroethylene reactor of volume 30mL, add each 10mL of absolute ethyl alcohol and DMF, be uniformly mixed, then use the above-mentioned sputter of clean tweezers gripping
?the ITO electro-conductive glass sheet inclined side of metal Sn is put in the polytetrafluoroethylene reactor, make metal covering upward, reaction is 4 hours under 160 ℃, and product respectively washs 3 times with distilled water and absolute ethyl alcohol, 60 ℃ of dryings of constant temperature make the SnS film in the substrate of ITO electro-conductive glass sheet; In the clean polytetrafluoroethylene reactor of volume 30mL, add the 3mg ammonium persulfate as oxidant, add distilled water 20mL, stirring and dissolving, then be put in the SnS film inclined side of preparation in the polytetrafluoroethylene reactor,
120 ℃ are reacted 24 hours, product is respectively washed 3 times with distilled water and absolute ethyl alcohol, and 60 ℃ of constant temperature are drying to obtain SnO
2film.Product is white transparent membrane, and the microstructure under scanning electron microscopy is the open structure that size particles is evenly distributed, and scanning electron micrograph is shown in Fig. 2.
embodiment 3:
1, preparation: volume 30mL polytetrafluoroethylene reactor is respectively washed 2 times with running water, distilled water, absolute ethyl alcohol successively, dry rear stand-by; Utilize magnetron sputtering sputter in the substrate of ITO electro-conductive glass
200nmthick metal Sn is stand-by.
2, reactions steps: add 3mg sulphur powder in the clean polytetrafluoroethylene reactor of volume 30mL, add each 10mL of a certain amount of absolute ethyl alcohol and DMF, be uniformly mixed, then use the above-mentioned sputter of clean tweezers gripping
?the ITO electro-conductive glass sheet inclined side of metal Sn is put in the polytetrafluoroethylene reactor, make metal covering upward, reaction is 4 hours under 160 ℃, and product respectively washs 3 times with distilled water and absolute ethyl alcohol, 60 ℃ of dryings of constant temperature make the SnS film standby in the substrate of ITO electro-conductive glass sheet; In the clean polytetrafluoroethylene reactor of volume 30mL, add the 3mg ammonium persulfate as oxidant, add distilled water 20mL, stirring and dissolving, then be put in the SnS film inclined side of preparation in its polytetrafluoroethylene reactor,
140 ℃ are reacted 24 hours, product is respectively washed 3 times with distilled water and absolute ethyl alcohol, and 60 ℃ of constant temperature are drying to obtain SnO
2the film product.Product is white transparent membrane, and the microstructure under scanning electron microscopy is the open structure that size particles is evenly distributed, and scanning electron micrograph is shown in Fig. 3, and X ray diffracting spectrum is shown in Fig. 4.
3, SnO
2the preparation of the hetero-junction thin-film solar cell device of/P3HT hydridization: utilize spin-coating method that the poly-3-hexyl thiophene conjugated polymer (P3HT) of the 10mg/mL for preparing is spun on to prepared SnO in vacuum glove box
2film surface, 120 ℃ of annealing in process 2 hours, finally utilize the vacuum evaporation instrument to steam and do electrode with Al, assembles to obtain ITO/SnO
2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.Fig. 5 is shown in by device assembling schematic diagram.
The photoelectric properties of assembled battery are tested by solar simulator, AM1.5 filter, 100 mW/cm
2xenon source irradiated, the density of photocurrent-voltage curve (I-V curve) that obtains battery is shown in Fig. 6.The open circuit voltage of this battery (Voc) is 0.405V, and density of photocurrent (Jsc) is 0.321mA/cm
2, fill factor, curve factor (FF) is 15.52%, the electricity conversion of this battery is 0.02% at present.
Claims (5)
1. the hetero-junction thin-film solar cell device of inorganic/organic hybrid, is characterized in that, it is ITO/SnO
2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.
As claimed in claim 1 a kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid, it is characterized in that: SnO wherein
2nano film material original position at low temperatures prepares, and method is with nanometer Sn
(0)for Xi Yuan, in the ITO electro-conductive glass substrate that is coated with metallic tin, by hydro-thermal and solvent heat two step wet chemicals, synthesize SnO
2nano film material, this thin-film material thickness is regulated and controled by reaction temperature and reaction time condition.
As claimed in claim 2 a kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid, it is characterized in that: SnO wherein
2the nano film material method that at low temperatures prepared by original position is, at first utilize magnetron sputtering sputter layer of metal tin in the substrate of ITO electro-conductive glass, by this sputter the ITO electro-conductive glass sheet inclined side of layer of metal tin be put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then add each 10mL of absolute ethyl alcohol and DMF, be placed at 160 ℃ of temperature solvent thermal reaction 4 hours, product uses distilled water and absolute ethanol washing more than 2 times, is drying to obtain the SnS film standby; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add the 3mg ammonium persulfate as oxidant, with the distillation water as solvent, the volume of distilled water is vessel volume 1/2~2/3, in temperature, be to react 24 hours at 140 ℃ of temperature, product uses distilled water and absolute ethanol washing more than 2 times, and drying at room temperature obtains SnO
2nano film material.
As claimed in claim 1 a kind of inorganic/the hetero-junction thin-film solar cell device of organic hybrid, it is characterized in that: SnO wherein
2with the preparation method of P3HT hybrid heterojunctions thin-film solar cells, be, at first utilize magnetron sputtering sputter layer of metal tin in the substrate of ITO electro-conductive glass, by this sputter the ITO electro-conductive glass sheet inclined side of layer of metal tin be put in volume 30mL polytetrafluoroethylene reactor, make metal covering upward, add 3mg sulphur powder, then add each 10mL of absolute ethyl alcohol and DMF, be placed at 160 ℃ of temperature solvent thermal reaction 4 hours, product uses distilled water and absolute ethanol washing more than 2 times, is drying to obtain the SnS film standby; Then the SnS film inclined side of preparation is put in 30mL polytetrafluoroethylene reactor, add the 3mg ammonium persulfate as oxidant, with the distillation water as solvent, the volume of distilled water is vessel volume 1/2-2/3, in temperature, be to react 24 hours at 140 ℃ of temperature, product uses distilled water and absolute ethanol washing more than 2 times, and drying at room temperature obtains SnO
2nano thin-film;
Then in vacuum glove box, utilize spin-coating method that the P3HT of the 10mg/mL for preparing is spun on to prepared SnO
2the nano thin-film surface, 120 ℃ of annealing in process 2 hours and get final product.
As claimed in claim 1 a kind of inorganic/preparation method of the hetero-junction thin-film solar cell device of organic hybrid, it is characterized in that: first by the step described in claim 4, prepare SnO
2with P3HT hybrid heterojunctions thin-film solar cells, recycling vacuum evaporation instrument steams does electrode with Al, assembles to obtain ITO/SnO
2: P3HT/Al is inorganic/the hetero-junction thin-film solar cell device of organic hybrid.
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CN105006370A (en) * | 2015-06-23 | 2015-10-28 | 南京航空航天大学 | Method for in-situ preparing CZTS counter electrode by means of solvent thermal and application of CZTS counter electrode |
CN105200523A (en) * | 2015-08-28 | 2015-12-30 | 内蒙古工业大学 | Method for synthesizing CdSe/P3HT composite nanocrystals by direct growth method |
CN111505062A (en) * | 2020-04-27 | 2020-08-07 | 电子科技大学 | Photovoltaic self-driven flexible gas sensor based on organic-inorganic heterojunction and preparation method thereof |
CN113097646A (en) * | 2021-04-09 | 2021-07-09 | 宁波合复新材料科技有限公司 | Preparation method of lithium-sulfur battery diaphragm |
CN115884611A (en) * | 2023-02-23 | 2023-03-31 | 北京科技大学 | CsPbI 3 Perovskite solar cell and preparation method thereof |
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CN105006370A (en) * | 2015-06-23 | 2015-10-28 | 南京航空航天大学 | Method for in-situ preparing CZTS counter electrode by means of solvent thermal and application of CZTS counter electrode |
CN105200523A (en) * | 2015-08-28 | 2015-12-30 | 内蒙古工业大学 | Method for synthesizing CdSe/P3HT composite nanocrystals by direct growth method |
CN111505062A (en) * | 2020-04-27 | 2020-08-07 | 电子科技大学 | Photovoltaic self-driven flexible gas sensor based on organic-inorganic heterojunction and preparation method thereof |
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CN115884611A (en) * | 2023-02-23 | 2023-03-31 | 北京科技大学 | CsPbI 3 Perovskite solar cell and preparation method thereof |
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