CN113937226A - Preparation method of perovskite material layer and perovskite solar cell - Google Patents
Preparation method of perovskite material layer and perovskite solar cell Download PDFInfo
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- CN113937226A CN113937226A CN202111203188.6A CN202111203188A CN113937226A CN 113937226 A CN113937226 A CN 113937226A CN 202111203188 A CN202111203188 A CN 202111203188A CN 113937226 A CN113937226 A CN 113937226A
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- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 238000000151 deposition Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 9
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 8
- JTDNNCYXCFHBGG-UHFFFAOYSA-L tin(ii) iodide Chemical compound I[Sn]I JTDNNCYXCFHBGG-UHFFFAOYSA-L 0.000 claims abstract description 6
- -1 amine halide Chemical class 0.000 claims abstract description 5
- 238000000859 sublimation Methods 0.000 claims abstract description 4
- 230000008022 sublimation Effects 0.000 claims abstract description 4
- 150000001412 amines Chemical class 0.000 claims abstract description 3
- QWANGZFTSGZRPZ-UHFFFAOYSA-N aminomethylideneazanium;bromide Chemical compound Br.NC=N QWANGZFTSGZRPZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- QHJPGANWSLEMTI-UHFFFAOYSA-N aminomethylideneazanium;iodide Chemical compound I.NC=N QHJPGANWSLEMTI-UHFFFAOYSA-N 0.000 claims abstract description 3
- ISWNAMNOYHCTSB-UHFFFAOYSA-N methanamine;hydrobromide Chemical compound [Br-].[NH3+]C ISWNAMNOYHCTSB-UHFFFAOYSA-N 0.000 claims abstract description 3
- LLWRXQXPJMPHLR-UHFFFAOYSA-N methylazanium;iodide Chemical compound [I-].[NH3+]C LLWRXQXPJMPHLR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000012808 vapor phase Substances 0.000 claims abstract description 3
- 230000005525 hole transport Effects 0.000 claims description 17
- 239000000758 substrate Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 230000031700 light absorption Effects 0.000 claims description 11
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000004549 pulsed laser deposition Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 239000000843 powder Substances 0.000 abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 238000000576 coating method Methods 0.000 description 7
- 239000010408 film Substances 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229920000144 PEDOT:PSS Polymers 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 239000000969 carrier Substances 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 125000003003 spiro group Chemical group 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910005855 NiOx Inorganic materials 0.000 description 1
- 229920001167 Poly(triaryl amine) Polymers 0.000 description 1
- XDLSXXMJBCNXPS-UHFFFAOYSA-N [Pb].CN Chemical compound [Pb].CN XDLSXXMJBCNXPS-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- 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 provides a preparation method of a perovskite material layer, which comprises the following steps: carrying out vapor phase sublimation on the raw material by adopting a pulse laser deposition method, and then depositing to obtain a perovskite material layer; the raw material is selected from perovskite single crystal or mixture; the mixture is a mixture of iodide and amine halide; the iodide is selected from PbI2Or SnI2(ii) a The halogenated amine is selected from one or more of methylamine iodide, methylamine bromide, formamidine iodide and formamidine bromide; the thickness of the perovskite material layer is 100-1000 nm. According to the invention, a perovskite crystal or a perovskite powder raw material of a specific kind is prepared by adopting a pulse laser deposition method to obtain a perovskite material layer, and the solar cell assembled by the perovskite material layer has higher photoelectric conversion efficiency.
Description
Technical Field
The invention belongs to the technical field of perovskite materials, and particularly relates to a preparation method of a perovskite material layer and a perovskite solar cell.
Background
Perovskite materials are widely applied to photoelectric devices due to the advantages of long carrier diffusion length, high carrier mobility, high photoluminescence quantum yield and the like, and in addition, the characteristics of solution processability and printability enable the perovskite materials to have good application prospects in commercial flexible devices.
The perovskite thin film prepared by the solution method in the prior art has some defects, such as vacancies, substitutional site atoms, grain boundaries and the like, which cause the performance of the battery to be reduced.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a perovskite material layer and a perovskite solar cell, wherein the perovskite material layer assembled cell prepared by the method has high photoelectric conversion efficiency.
The invention provides a preparation method of a perovskite material layer, which comprises the following steps:
carrying out vapor phase sublimation on the raw material by adopting a pulse laser deposition method, and then depositing to obtain a perovskite material layer;
the raw material is selected from perovskite single crystal or mixture; the mixture is a mixture of iodide and amine halide; the iodide is selected from PbI2Or SnI2(ii) a The halogenated amine is selected from one or more of methylamine iodide, methylamine bromide, formamidine iodide and formamidine bromide;
the thickness of the perovskite material layer is 100-1000 nm.
In the invention, the perovskite single crystal is an organic-inorganic hybrid methylamine lead iodoperovskite single crystal which is purchased from Xianbaolite photoelectric technology Limited.
In the invention, the laser wavelength adopted by the pulse laser deposition method is 193nm, the single pulse energy is 100-400 mJ, the target spacing is 10-50 cm, the pulse frequency is 50-300 kHz, the substrate temperature is 0-300 ℃, and the vacuum degree is 1 multiplied by 10-5～1×10-1Pa。
In the invention, the mass ratio of the iodide to the amine halide is (1:3) to (3: 1);
the particle size of the mixture is 50-1000 nm.
In the present invention, the composition of the perovskite material layer is selected from MAPbI3。
The invention provides a perovskite solar cell, which comprises a conductive electrode substrate layer, a hole transport layer, a perovskite light absorption layer, an electron transport layer and a metal electrode layer which are sequentially arranged;
or comprises a conductive electrode substrate layer, an electron transport layer, a perovskite light absorption layer, a hole transport layer and a metal electrode layer which are arranged in sequence;
the perovskite light absorption layer is a perovskite material layer prepared by the method in the technical scheme.
In the present invention, the conductive electrode base layer is preferably an FTO transparent electrode; before the conductive electrode is used, preferably, deionized water, acetone and isopropanol are sequentially adopted to perform ultrasonic treatment for 10-20 min respectively, then an ultraviolet light cleaning machine is adopted to clean for 8-12 min, and nitrogen flow is blown for drying for later use.
The hole transport layer is prepared on the conductive electrode substrate layer by adopting a scraper coating method. In a specific embodiment of the present invention, the hole transport layer is preferably a commercially available PEDOT: PSS (AI4083) in aqueous solution; the invention preferably adopts isopropanol in a volume ratio of 1:3, proportioning and diluting, wherein the coating speed of a scraper is 10-20 mm/s, and preferably 15 mm/s; the coating temperature is 45-70 ℃, and preferably 55 ℃; the distance between the scraper and the substrate is 45-55 mu m, preferably 50 mu m; annealing in nitrogen after coating, wherein the annealing temperature is 80-100 ℃, and preferably 90 ℃; the annealing time is 10-20 min, preferably 15 min.
The electron transport layer is preferably prepared by an evaporation method, and the evaporation speed is 0.1-0.5A/s, preferably 0.3A/s. The metal electrode layer is preferably prepared in a vapor deposition mode; the speed of the vapor deposition is 0.1-0.5A/s, preferably 0.3A/s.
In the present invention, if the conductive electrode base layer contacts the hole transport layer; the raw material of the hole transport layer comprises PEDOT: PSS (AI4083) aqueous solution, NiOxPTAA or Spiro; the raw materials for preparing the electron transport layer comprise C60 and SnO2Or TiO2。
In the invention, if the conductive electrode substrate layer contacts with the electron transport layer, the raw materials of the electron transport layer comprise C60 and SnO2Or TiO2(ii) a The raw material of the hole transport layer is PTAA or Spiro;
in the invention, the metal electrode layer adopts one or more metal electrodes selected from Cu, Al, Au and Ag.
The thickness of the hole transport layer is 20-100 nm; in a specific embodiment, the hole transport layer has a thickness of 100 nm. The thickness of the electron transmission layer is 20-100 nm, and preferably 40-50 nm; in a specific embodiment, the thickness of the electron transport layer is 45 nm. The thickness of the metal electrode layer is 80-300 nm, and preferably 100 nm; in a specific embodiment, the metal electrode material is preferably copper; the thickness of the metal electrode layer is 100 nm.
In the invention, the thickness of the perovskite light absorption layer is 100-1000 nm; in a specific embodiment, the thickness of the perovskite light absorption layer is 350 nm.
The invention adopts the pulse laser deposition method to prepare the perovskite crystal or the perovskite powder raw material of specific type to obtain the perovskite material layer, and the solar cell device assembled by the perovskite material layer has higher photoelectric conversion efficiency.
Through the method of GB/T6495.1-1996, the invention passes through the original table of Gekkili 2400, and standard light (100mW cm) is generated at AM1.5G-2) Next, the J-V curve of the perovskite solar cell was tested using a (Newport, Class 3A),84023A solar simulator.
Drawings
Fig. 1 is a schematic structural diagram of a perovskite-type solar device provided by the present invention, wherein 102 is a conductive electrode substrate layer, 104 is a hole transport layer (or an electron transport layer), 106 is a perovskite material layer, 108 is an electron transport layer (or a hole transport layer), and 110 is a metal electrode layer;
FIG. 2 is a scanning electron micrograph of a cross-section of a perovskite layer prepared in example 1;
FIG. 3 is a scanning electron micrograph of a section of a perovskite layer prepared in the control group.
Detailed Description
In order to further illustrate the present invention, the following will describe in detail the preparation method of a perovskite material layer and the perovskite solar cell provided by the present invention with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Fig. 1 is a schematic structural diagram of the perovskite type solar device, and the structure of the perovskite type solar device is composed of the following parts:
1. conductive electrode substrate 102: taking the substrate deposited on the transparent FTO transparent electrode as the device as an example, the area of the substrate is not limited (5X 5cm in this example)2) The product can be directly used as a commercialized product with large-scale mass production. Before use, the surface of the electrode is sequentially treated by deionized water, acetone and isopropanol for 15 minutes and then cleaned by an ultraviolet light cleaner for 10 minutes, and nitrogen is addedAnd (5) drying by air flow for later use.
2. On the conductive electrode substrate, the obtained hole transport layer 104 was prepared by a doctor blade coating method using a slurry of commercial PEDOT: PSS (AI4083) in aqueous solution, using isopropanol, in a volume ratio of 1:3, diluting in proportion, wherein the coating speed of a scraper is 15 mm/s; the coating temperature is 55 ℃; the distance between the scraper and the substrate is 50 mu m; after coating, annealing at 90 ℃ for 15 minutes in nitrogen to obtain a hole transport layer with a thickness of 100 nm.
3. The perovskite light absorption layer 106 prepared on the hole transport layer has the structure of MAPbI3. Depositing an organic-inorganic hybrid methylamine lead-iodoperovskite monocrystal (which can be purchased commercially) by adopting pulsed laser deposition and then depositing to form a perovskite material layer;
wherein the laser wavelength is 193nm, the single pulse energy is 200mJ, the target spacing is 20cm, the pulse frequency is 100Khz, the substrate temperature is 150 ℃, and the vacuum degree is 1 multiplied by 10-4Pa；
a) The thickness of the prepared perovskite material layer is 350 nm;
b) the thickness of the prepared perovskite material layer is 2000 nm;
4. and the electron transport layer 108 is prepared on the perovskite light absorption layer by a thermal evaporation method, and is made of C60. The evaporation speed is 0.3A/s; the thickness was 45 nm.
5. The metal electrode layer 110 is evaporated on the electron transport layer and is made of high-purity copper (> 99.99%). The evaporation speed is 0.3A/s; the thickness of the copper film was 100 nm.
The sections of the perovskite layers prepared in the embodiment 1 and the control group are tested by a ZEISS Sigma 300 field emission scanning electron microscope, as shown in figures 2 and 3 respectively, and as can be seen from figure 2, the film grain boundary is obvious and is communicated up and down at 350nm, so that the longitudinal transportation of current carriers can be ensured, the interface recombination caused by film delamination and the like is reduced, and the photoelectric conversion efficiency is better; as can be seen in fig. 3: the thickness of the perovskite film layer prepared by a vapor sputtering method is about 2000nm, and the free path of perovskite current carriers is about 1 mu m, so that the prepared film has a better structure, namely the film is vertically through and has no obvious crystal boundary, but the thicker film influences the effective transmission and extraction of the photon-generated current carriers, and the efficiency of the obtained perovskite battery is lower.
a) The perovskite solar cell prepared with the perovskite light absorbing layer 106 of the set is designated as example 1;
b) perovskite light absorbing layer 106 of set perovskite solar cells prepared were noted as a control.
The photoelectric conversion efficiency of the perovskite solar cell prepared by the example 1 and the control group is 14% and 0.35%.
Example 2
Unlike example 1, the single pulse energy was 400 mJ.
The photoelectric conversion efficiency of the perovskite solar device assembled by the perovskite light absorption layer prepared in example 2 is 6.5%.
Example 3
The difference from example 1 is that the perovskite material layer is produced according to the following method:
mixing MAI powder and PbI in a molar ratio of 1:12Mixing, namely taking corundum ceramic balls as grinding balls, filling the mixed powder into a ball milling tank, and putting the ball milling tank on a GMS5-8 type horizontal ball mill for ball milling to obtain MAPbI3The powder of (4). MAPbI obtained after ball milling3The powder was dry-pressed in a YP15A type powder press.
MAPbI to be shaped using pulsed laser deposition3Depositing the powder after vapor sublimation to form a perovskite material layer;
wherein the laser wavelength is 193nm, the single pulse energy is 200mJ, the target spacing is 20cm, the pulse frequency is 100Khz, the substrate temperature is 150 ℃, and the vacuum degree is 1 multiplied by 10-4Pa；
The thickness of the prepared perovskite material layer is 350 nm.
The photoelectric conversion efficiency of the perovskite solar device assembled by the perovskite material layer prepared in example 3 is 11.2%.
According to the embodiment, the perovskite material layer is prepared by adopting the pulse laser deposition method to prepare the perovskite crystal or the perovskite powder raw material of the specific type, and the solar cell device assembled by the perovskite material layer has high photoelectric conversion efficiency.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A method of producing a layer of perovskite material, comprising the steps of:
carrying out vapor phase sublimation on the raw material by adopting a pulse laser deposition method, and then depositing to obtain a perovskite material layer;
the raw material is selected from perovskite single crystal or mixture; the mixture is a mixture of iodide and amine halide; the iodide is selected from PbI2Or SnI2(ii) a The halogenated amine is selected from one or more of methylamine iodide, methylamine bromide, formamidine iodide and formamidine bromide;
the thickness of the perovskite material layer is 100-1000 nm.
2. The method according to claim 1, wherein the pulsed laser deposition method uses a laser wavelength of 193nm, a single pulse energy of 100 to 400mJ, a target gap of 10 to 50cm, a pulse frequency of 50 to 300kHz, a substrate temperature of 0 to 300 ℃ and a degree of vacuum of 1X 10-5～1×10-1Pa。
3. The production method according to claim 1, wherein the mass ratio of the iodide to the amine halide is (1:3) to (3: 1);
the particle size of the mixture is 50-1000 nm.
4. The method of claim 1, wherein the perovskite material layer has a composition selected from MAPbI3。
5. The perovskite solar cell is characterized by comprising a conductive electrode substrate layer, a hole transport layer, a perovskite light absorption layer, an electron transport layer and a metal electrode layer which are sequentially arranged;
or comprises a conductive electrode substrate layer, an electron transport layer, a perovskite light absorption layer, a hole transport layer and a metal electrode layer which are arranged in sequence;
the perovskite light absorption layer is a perovskite material layer prepared by the method of any one of claims 1 to 4.
6. The perovskite solar cell according to claim 5, wherein the hole transport layer has a thickness of 20 to 100 nm;
the thickness of the electron transmission layer is 20-100 nm.
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| CN105900255A (en) * | 2013-09-10 | 2016-08-24 | 洛桑联邦理工学院 | Inverted solar cell and process for producing the same |
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| CN115032209A (en) * | 2022-08-11 | 2022-09-09 | 中国华能集团清洁能源技术研究院有限公司 | Quality detection method for transparent conductive film |
| CN115032209B (en) * | 2022-08-11 | 2022-11-15 | 中国华能集团清洁能源技术研究院有限公司 | Quality detection method for transparent conductive film |
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Application publication date: 20220114 |
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