CN108321299B - Low-dimensional lead-free perovskite thin film and preparation method of lead-free perovskite solar cell - Google Patents
Low-dimensional lead-free perovskite thin film and preparation method of lead-free perovskite solar cell Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000010409 thin film Substances 0.000 title claims abstract description 17
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000004528 spin coating Methods 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000012046 mixed solvent Substances 0.000 claims abstract description 9
- 230000005540 biological transmission Effects 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000000137 annealing Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 9
- MCEWYIDBDVPMES-UHFFFAOYSA-N [60]pcbm Chemical compound C123C(C4=C5C6=C7C8=C9C%10=C%11C%12=C%13C%14=C%15C%16=C%17C%18=C(C=%19C=%20C%18=C%18C%16=C%13C%13=C%11C9=C9C7=C(C=%20C9=C%13%18)C(C7=%19)=C96)C6=C%11C%17=C%15C%13=C%15C%14=C%12C%12=C%10C%10=C85)=C9C7=C6C2=C%11C%13=C2C%15=C%12C%10=C4C23C1(CCCC(=O)OC)C1=CC=CC=C1 MCEWYIDBDVPMES-UHFFFAOYSA-N 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 229920000144 PEDOT:PSS Polymers 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 6
- JTDNNCYXCFHBGG-UHFFFAOYSA-L tin(ii) iodide Chemical compound I[Sn]I JTDNNCYXCFHBGG-UHFFFAOYSA-L 0.000 claims description 6
- DDQAGDLHARKUFX-UHFFFAOYSA-N acetic acid;methanamine Chemical compound [NH3+]C.CC([O-])=O DDQAGDLHARKUFX-UHFFFAOYSA-N 0.000 claims description 5
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- RAJISUUPOAJLEQ-UHFFFAOYSA-N chloromethanamine Chemical compound NCCl RAJISUUPOAJLEQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 229940108184 stannous iodide Drugs 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- 238000000280 densification Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 229960002358 iodine Drugs 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 claims description 2
- 229960002799 stannous fluoride Drugs 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000012296 anti-solvent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 231100000701 toxic element Toxicity 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000003940 butylamines Chemical class 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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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
- H10K30/20—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising organic-organic junctions, e.g. donor-acceptor junctions
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
-
- 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
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Abstract
The invention relates to a low-dimensional lead-free perovskite thin film and a preparation method of a lead-free perovskite solar cell thereof, belonging to the field of photoelectric materials and devices. The invention utilizes special mixed solvent and heating spin coating technology to prepare the low-dimensional tin-based perovskite thin film on the ITO glass substrate deposited with the hole transmission layer by one-step spin coating, and after annealing treatment, the thin film has a smooth and compact surface, the grain size is close to 10 mu m, and the preparation method is simple and easy. The prepared low-dimensional tin-based perovskite solar cell has high photoelectric conversion efficiency and good device stability.
Description
Technical field
The present invention relates to a kind of low-dimensionals without lead-based perovskite film and its unleaded perovskite preparation method of solar battery, especially
It is that one kind can prepare the unleaded perovskite thin film of high quality low-dimensional of super large crystal grain and its straightforward procedure of solar cell device,
Belong to photoelectric material and device arts.
Background technique
With the continuous development of society, energy pollution problem is increasingly valued by people, and finds cleaning renewable energy
Source and extremely urgent.Solar energy is concerned by people as one of renewable energy the most abundant on the earth.Wherein, too
Positive energy battery is an important channel using solar energy.What existing market used is silicon solar cell mostly, but silicon
Solar battery higher cost, energy consumption is high, largely limits the large-scale application of silicon solar cell.
Hybrid inorganic-organic perovskite solar battery came out so far from 2009, and a few years incident photon-to-electron conversion efficiency is just
It is promoted from 3.8% to 22.7%.Although the incident photon-to-electron conversion efficiency development of perovskite solar battery is so rapid, in its production
Many problems are still remained in the reason of industry.Wherein, the organic inorganic hybridization perovskite solar battery generally used
All there is two urgent problems when market-oriented.One is exactly that toxic element lead is badly in need of replacement, another is exactly
Perovskite external environment job stability has to be hoisted.
Tin element is generally all used for the replacement of toxic element lead at present, but in air easily due to divalent tin element
Oxidation, causes its device very unstable.Although there is the method for using for reference lead-based perovskite solar cell stability to prepare at present
Low-dimensional tin based perovskites film and its solar battery make its stability obtain certain promotion, but since its film crystallized
The bad control of journey causes its film quality not high.And big Alternative uses anti-solvent, increase preparation process complexity and
Cost.The solvent effect of present invention combination Special Mixed solvent and simple step heating spin-coating method control low-dimensional well
The crystallization process of tin based perovskites film has obtained the low-dimensional tin based perovskites film of high quality super large crystal grain.And final
Device performance and stability have certain promotion.
Summary of the invention
Present invention solves the technical problem that being, film quality not easy to control for low-dimensional tin based perovskites crystallization of thin films
It is not high, propose a kind of simple super large crystal grain, the unleaded perovskite thin film of low-dimensional and its unleaded perovskite solar battery preparation side
Method.
In order to solve the above-mentioned technical problem, technical solution proposed by the present invention is: a kind of simple, super large crystal grain, low
Tie up unleaded perovskite thin film and its unleaded perovskite preparation method of solar battery, comprising the following steps:
(1) by the salt compounded of iodine of butylamine, chloromethane amine, stannous iodide and stannous fluoride in molar ratio 2:3:4:0.8 be dissolved in it is special
In the mixed solvent be configured to low-dimensional tin based perovskites precursor liquid, stirred 3-5 hours at 30-120 DEG C；
(2) the spin-on deposition hole mobile material in cleaning and processed transparent electro-conductive glass；
(3) thin using heating spin coating technique deposition low-dimensional tin based perovskites in the ITO substrate for being deposited with hole transmission layer
Film obtains the super large crystal grain tin based perovskites film of smooth densification after annealing；
(4) the spin-on deposition electron transfer layer on this perovskite thin film；
(5) then vacuum thermal evaporation interface-modifying layer and metal electrode on the electron transport layer.
Preferably, mixed solvent special in the step (1) is the mixed solvent of acetic acid methylamine and dimethyl sub-maple,
Acetic acid methylamine volume ratio dimethyl sub-maple volume is 25%-400% in 3.
Preferably, perovskite Concentration of precursor solution is 100-300mg/mL in the step (1).
Preferably, the hole transmission layer deposited in electrically conducting transparent ITO electrode in the step (2) is PEDOT:PSS, specifically
Step are as follows: after spin coating PEDOT:PSS, anneal 30min at 120 DEG C.
Preferably, the substrate temperature of heating spin coating technique is 40-120 DEG C in the step (3).
Preferably, the electron transfer layer of spin-on deposition is PCBM in the step (4), and wherein PCBM is with the dense of 18mg/mL
Degree is dissolved in chlorobenzene solution.
Preferably, step (5) the median surface decorative layer is LiF, metal electrode Al.Specific steps are as follows:
(1) LiF hot evaporation on the electron transport layer, with a thickness of 1nm.
(2) metal Al thickness of electrode is 100nm.
To solve the above-mentioned problems, proposed by the present invention another solution is that the unleaded perovskite thin film of the low-dimensional
And its perovskite solar battery of unleaded perovskite preparation method of solar battery preparation.
To solve the above-mentioned problems, proposed by the present invention another solution is that the unleaded perovskite thin film of the low-dimensional
And its application of the perovskite solar battery of unleaded perovskite preparation method of solar battery preparation in photoelectric field.
Beneficial effects of the present invention:
(1) low-dimensional is controlled well using the solvent effect of proper proportion acetic acid methylamine and dimethyl sub-maple mixed solvent
The crystallization process of tin based perovskites film has obtained the perovskite thin film of high quality super large crystal grain (grain size is about 10 μm)；
(2) use for heating spin coating technique controls low-dimensional tin based perovskites film normal well and grows in substrate, and one
Determine to improve carrier mobility and device performance in degree；
The heating spin coating of (3) one steps is not only easy to operate compared to anti-solvent method, and cost also has reduction to a certain extent；
(4) spin coating low-dimensional tin based perovskites solar battery, light can also be prepared in air using method of the invention
Electrotransformation efficiency > 1.2%；
(5) the tin based perovskites solar cell device performance and stability prepared in nitrogen atmosphere has significantly
It is promoted.
Detailed description of the invention
Of the invention is described further with reference to the accompanying drawing.
Fig. 1 is the SEM figure of the low-dimensional tin based perovskites film for the super large crystal grain that the present invention is prepared in nitrogen atmosphere；
Fig. 2 is low-dimensional tin based perovskites solar cell device structure chart prepared by the present invention；
Fig. 3 is the J-V curve graph for the low-dimensional tin based perovskites solar battery that the present invention is prepared in nitrogen atmosphere；
Fig. 4 is that photoelectricity of the low-dimensional tin based perovskites solar battery of the invention being prepared in nitrogen encapsulation turns
Change efficiency versus time curve；
Fig. 5 is the low-dimensional tin based perovskites film change of film XRD at any time under external environment that the present invention is prepared
Change figure；
Fig. 6 is the J-V curve for the low-dimensional tin based perovskites solar cell device that the present invention is prepared in air；
Specific embodiment
Embodiment
The present embodiment is the unleaded perovskite thin film of super large crystal grain low-dimensional invented and its unleaded perovskite solar battery system
The inversion planar heterojunction solar battery of Preparation Method preparation mainly comprises the steps that fully understand the present invention
Step 1) by the ITO electro-conductive glass etched successively ethyl alcohol, ultrapure water add cleaning agent, ultrapure water, in ethyl alcohol it is each
Ultrasonic 30min.It is put into baking oven baking after being dried with nitrogen, obtains clean ITO substrate.
Step 2) weighs 38.37mg butylamine salt compounded of iodine, 19.34mg chloromethane amine, 142.29mg stannous iodide and 11.97mg fluorination
Stannous is dissolved in the in the mixed solvent of acetic acid methylamine and dimethyl sub-maple, and stirs 4 hours to being completely dissolved at 60 DEG C, is prepared into
Perovskite precursor solution, concentration 200mg/mL.
Step 4) handles the ITO substrate UV ozone cleaned up in step 1) 15 minutes.
Step 5) takes 50 μ L of hole mobile material PEDOT:PSS to drop to the ITO conduction glass that step 4) is handled well with liquid-transfering gun
On glass, will be coated with PEDOT:PSS after rotating 50 seconds under 5000 rpms of revolving speed 120 DEG C of ITO under the conditions ofs, anneal
30min。
The ITO conductive substrate for being coated with hole transmission layer that annealing is completed in step 5) is placed on heating spin coating instrument by step 6)
On, preheat 3min.
The 75 μ L of perovskite precursor solution that step 7) takes step 3) to prepare is dripped on the ITO substrate of step 6) preheating, rotation
Film forming is applied, then anneals, obtains perovskite thin film.The revolving speed of spin coating perovskite precursor solution rotates for per minute 4000
It applies 20 seconds, anneal 5min in nitrogen atmosphere.
Step 8) weighs 18mg PCBM, is dissolved completely in 1ml chlorobenzene solvent, and the PCBM rotation of 18mg/mL is configured to
Masking liquid.
The PCBM spin coating liquid of step 8) is spun on the perovskite thin film of step 7) by step 9), and spin coating PCBM uses every point
Clock 1000 rotates painting 60 seconds, obtains electron transfer layer.
Step 10) uses vacuum thermal evaporation technology, and 1nm LiF and 100nm gold are deposited on the electron transfer layer of step 9)
Belong to electrode A l, obtains perovskite solar battery.
Step 11) (AM1.5G illumination) under standard test condition, the light of solar cell device prepared by this example
Photoelectric transformation efficiency is 3.17%, open-circuit voltage 0.34V, short circuit current 17.63mA/cm2, fill factor 52.84%.
Of the invention is not limited to the above embodiment the specific technical solution, all technologies formed using equivalent replacement
Scheme be the present invention claims protection scope.
Claims (8)
1. a kind of unleaded perovskite preparation method of solar battery of low-dimensional, which comprises the following steps:
(1) by the salt compounded of iodine of butylamine, chloromethane amine, 2:3:4:0.8 is dissolved in special mix in molar ratio for stannous iodide and stannous fluoride
It is configured to low-dimensional tin based perovskites precursor liquid in bonding solvent, is stirred 3-5 hours at 30-120 DEG C；
(2) the spin-on deposition hole mobile material in cleaning and processed transparent electro-conductive glass；
(3) in the ITO substrate for being deposited with hole transmission layer, low-dimensional tin based perovskites film is deposited using heating spin coating technique,
The super large crystal grain tin based perovskites film of smooth densification is obtained after annealing；
(4) the spin-on deposition electron transfer layer on this perovskite thin film；
(5) then vacuum thermal evaporation interface-modifying layer and metal electrode on the electron transport layer；
Special mixed solvent is the mixed solvent of acetic acid methylamine and dimethyl sub-maple in the step (1), wherein tumer
Amine volume ratio dimethyl sub-maple volume is 25%-400%.
2. the unleaded perovskite preparation method of solar battery of low-dimensional according to claim 1, it is characterised in that: the step
Suddenly perovskite Concentration of precursor solution is 100-300mg/mL in (1).
3. the unleaded perovskite preparation method of solar battery of low-dimensional according to claim 1, it is characterised in that: the step
Suddenly the hole transmission layer deposited in electrically conducting transparent ITO electrode in (2) is PEDOT:PSS, specific steps are as follows: spin coating PEDOT:PSS
Afterwards, anneal 30min at 120 DEG C.
4. the unleaded perovskite preparation method of solar battery of low-dimensional according to claim 1, it is characterised in that: the step
Suddenly the substrate temperature of heating spin coating technique is 40-120 DEG C in (3).
5. the unleaded perovskite preparation method of solar battery of low-dimensional according to claim 1, it is characterised in that: the step
Suddenly the electron transfer layer of spin-on deposition is PCBM in (4), and wherein PCBM is dissolved in chlorobenzene solution with the concentration of 18mg/mL.
6. the unleaded perovskite preparation method of solar battery of low-dimensional according to claim 1, it is characterised in that: the step
Suddenly (5) median surface decorative layer is LiF, metal electrode Al, specific steps are as follows:
(1) LiF hot evaporation on the electron transport layer, with a thickness of 1nm；
(2) metal Al thickness of electrode is 100nm.
7. the perovskite that according to claim 1 prepared by -6 any unleaded perovskite preparation method of solar battery of the low-dimensional is too
Positive energy battery.
8. the perovskite solar-electricity of the unleaded perovskite preparation method of solar battery preparation of low-dimensional according to claim 7
Application of the pond in photoelectric field.
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| CN109378386B (en) * | 2018-10-16 | 2022-06-07 | 南京邮电大学 | Method for regulating morphology of lead-free perovskite solar cell and prepared cell device |
| CN110299455B (en) * | 2019-06-27 | 2022-08-02 | 南京邮电大学 | Preparation method for regulating surface morphology of lead-free perovskite solar cell |
| CN111952455B (en) * | 2020-08-17 | 2023-11-03 | 南京工业大学 | Preparation of low-dimensional stannyl perovskite film by ionic liquid type organic large-volume amine molecular salt, solar cell and application thereof |
| CN112542549B (en) * | 2020-12-08 | 2023-10-20 | 南京工业大学 | Wide-bandgap perovskite solar cell and preparation and application thereof |
| CN113192843B (en) * | 2021-04-06 | 2022-11-08 | 电子科技大学 | Preparation method and application of novel non-lead-based perovskite film |
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