CN114388697A - Hole transport layer precursor solution and preparation method and application thereof - Google Patents
Hole transport layer precursor solution and preparation method and application thereof Download PDFInfo
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- CN114388697A CN114388697A CN202111302517.2A CN202111302517A CN114388697A CN 114388697 A CN114388697 A CN 114388697A CN 202111302517 A CN202111302517 A CN 202111302517A CN 114388697 A CN114388697 A CN 114388697A
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- 230000005525 hole transport Effects 0.000 title claims abstract description 86
- 239000002243 precursor Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title description 14
- 239000003085 diluting agent Substances 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 36
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 238000004528 spin coating Methods 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 25
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 24
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 12
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 6
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 6
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 6
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- 229910005581 NiC2 Inorganic materials 0.000 claims description 3
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 claims description 3
- 229910021587 Nickel(II) fluoride Inorganic materials 0.000 claims description 3
- 229910021588 Nickel(II) iodide Inorganic materials 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 claims description 3
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims description 3
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 claims description 3
- FUFKFNZOGMJPAL-UHFFFAOYSA-N nickel(2+);hydrate Chemical compound O.[Ni+2] FUFKFNZOGMJPAL-UHFFFAOYSA-N 0.000 claims description 3
- 229910021508 nickel(II) hydroxide Inorganic materials 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(II) nitrate Inorganic materials [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 claims description 3
- DBJLJFTWODWSOF-UHFFFAOYSA-L nickel(ii) fluoride Chemical compound F[Ni]F DBJLJFTWODWSOF-UHFFFAOYSA-L 0.000 claims description 3
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 claims description 3
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 3
- PZFKDUMHDHEBLD-UHFFFAOYSA-N oxo(oxonickeliooxy)nickel Chemical compound O=[Ni]O[Ni]=O PZFKDUMHDHEBLD-UHFFFAOYSA-N 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- LFETXMWECUPHJA-UHFFFAOYSA-N methanamine;hydrate Chemical compound O.NC LFETXMWECUPHJA-UHFFFAOYSA-N 0.000 claims 1
- 239000010409 thin film Substances 0.000 abstract description 8
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 238000003980 solgel method Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 20
- 239000011521 glass Substances 0.000 description 18
- 230000031700 light absorption Effects 0.000 description 11
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000000137 annealing Methods 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 239000000969 carrier Substances 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 229910005855 NiOx Inorganic materials 0.000 description 5
- 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 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 239000012459 cleaning agent Substances 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 5
- 238000004506 ultrasonic cleaning Methods 0.000 description 5
- 238000007740 vapor deposition Methods 0.000 description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000004770 highest occupied molecular orbital Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 150000002816 nickel compounds Chemical class 0.000 description 2
- -1 nickel metal compound Chemical class 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000008033 biological extinction Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- MVPPADPHJFYWMZ-IDEBNGHGSA-N chlorobenzene Chemical group Cl[13C]1=[13CH][13CH]=[13CH][13CH]=[13CH]1 MVPPADPHJFYWMZ-IDEBNGHGSA-N 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
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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
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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
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
-
- 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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- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention relates to a hole transport layer precursor solution, comprising: a hole transport material, a first diluent, and a second diluent; wherein the hole transport material is a compound of metallic nickel and/or a complex of metallic nickel, and the molar concentration of the hole transport material is 0.02-10 mol/L; the volume ratio of the first diluent to the second diluent is 1: (0.1-1000). The hole transport layer precursor solution can obtain NiO with good crystallizationxThe trans-perovskite solar cell is good in crystallization and chemical stability, high in hole mobility and easy to prepare, can be applied to a trans-perovskite cell, can realize large-area lossless coating on the surface of a perovskite thin film, is better in performance and stability, and is easier for industrial production due to the fact that a hole transport layer of the trans-perovskite solar cell is prepared in a large area through a sol-gel method.
Description
Technical Field
The invention relates to the technical field of perovskite solar cells, in particular to a hole transport layer precursor solution and a preparation method and application thereof.
Background
In recent years, based on organic-inorganic metal halide perovskites (ABX)3) Have received a great deal of attention due to their unique physicochemical properties. The perovskite material has the advantages of high extinction coefficient, strong charge transfer capacity, long carrier service life, long carrier diffusion distance, special bipolarity and low cost and is easy to manufacture. From 2009 toNowadays, the photoelectric conversion efficiency of perovskite solar cells is increased from the first 3.8% to 25.8%, making it a new solar cell most likely to replace the conventional single crystalline silicon solar cell in the future.
The perovskite solar cell can be divided into an upright structure (n-i-p type) and an inverted structure (p-i-n type) on the device structure. In a typical structure, a conductive substrate, an electron transport layer, a perovskite light absorbing layer, a hole transport layer, and a metal electrode are included. When photons with energy larger than the forbidden band width of the perovskite are incident to the perovskite solar cell, the perovskite light absorption material is excited by light to generate excitons, and the excitons are separated in the material and at the interface to form conduction band electrons and valence band holes; subsequently, electrons and holes are injected into the conduction band of the electron transport material and the Highest Occupied Molecular Orbital (HOMO) of the hole transport material, respectively; and finally, the electrons injected into the conduction band of the electron transport material are collected by the conductive substrate and then are transmitted to an external circuit, and the holes in the hole transport layer flow to the external circuit through the metal electrode, so that a complete cycle is formed. Although the efficiency of the perovskite solar cell is developed in a leap-type manner, the perovskite solar cell still faces the key problems of poor stability, J-V delay, high cost and the like, and the commercial application of the perovskite solar cell is greatly limited.
At present, Spiro-OMe TAD is a hole transport material widely used in perovskite solar cells. However, there are also many disadvantages to the Spiro-OMe TAD, such as: (1) the synthesis process is complex, the parts are harsh, the purification is difficult, and the price is high; (2) the hole mobility is low, and a dopant (such as Li-TFSI) is required to be added to improve the hole transport performance of the perovskite solar cell so as to prepare a high-efficiency perovskite solar cell, but the dopant is extremely easy to deliquesce under an atmospheric environment to cause the degradation of the cell performance. The above disadvantages limit its large scale application in perovskite solar cells. Therefore, it is of great significance to develop a hole transport material with simple synthesis, low cost and good hole transport performance to replace the Spiro-OMe TAD.
Disclosure of Invention
The invention aims to provide a hole transport layer precursor solution, a preparation method and application thereof, aiming at the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
a first aspect of the present invention provides a hole transport layer precursor solution comprising: a hole transport material, a first diluent, and a second diluent;
wherein the hole transport material is a compound of metallic nickel and/or a complex of metallic nickel, and the molar concentration of the hole transport material is 0.02-10 mol/L; the volume ratio of the first diluent to the second diluent is 1: (0.1-1000).
Preferably, the hole transport material is selected from nickel (II) bis (2, 4-pentanedionate) hydrate, NiC2O4、NiSO4、NiSO4·7H2O、NiCO3、NiF2、NiBr2、NiI2、NiCl2·6H2O、NiCl2、Ni(OH)2、Ni(OH)3、Ni2O3、Ni(CO)4、(C2H5)2Ni、[Ni(NH3)6]Cl2、[Ni(CN)4]Cl2、Ni(NO3)2·H2O、[Ni(en)3]Cl2Or [ Ni (H) ]2O)6]Cl2At least one of (1).
Preferably, the first diluent is selected from at least one of methanol, acetonitrile, water, chlorobenzene, toluene, ethanol, dimethylformamide, dimethyl sulfoxide, acetone, isopropanol, ethyl acetate, ammonia water or aqueous methylamine solution.
Preferably, the second diluent is selected from at least one of ethanol, acetone, dioxane, tetrahydrofuran, methyl ethyl ketone, n-butanol, ethyl acetate, diethyl ether, isopropyl ether, dichloromethane, chloroform, bromoethane, benzene, carbon tetrachloride, carbon disulfide, cyclohexane and hexane.
A second aspect of the present invention provides a method for preparing a hole transport layer precursor solution as described above, comprising the steps of: and mixing the hole transport material, the first diluent and the second diluent, and performing dispersion treatment to obtain the hole transport layer precursor solution.
A third aspect of the present invention is to provide a hole transport layer prepared from the hole transport layer precursor solution as described above.
Preferably, the method for preparing the hole transport layer is at least one selected from spin coating, spray coating, blade coating, dipping, and slit coating.
A fourth aspect of the invention provides a trans-perovskite solar cell comprising: a conductive substrate, a hole transport layer, a perovskite light absorbing layer, an electron transport layer as described above, a blocking layer, and an electrode.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the hole transport layer precursor solution can be uniformly attached to FTO glass by methods such as spraying, spin coating and the like, and NiO uniformly covered can be obtained after annealingxThe hole transport layer can obtain NiO with better crystallization than other methodsxCrystallization, and at the same time, at high temperature, redundant water can be discharged, which is more beneficial to the transmission of current carriers and improves the transmission speed of the current carriers, thereby improving the photoelectric conversion efficiency of the perovskite solar cell; and NiOxHas good chemical stability, high hole mobility and easy preparation, compared with NiO prepared by using compounds to react with each otherxBecause the hole transport layer precursor solution of the invention only has a single nickel compound, the NiO prepared by the inventionxThe purity is higher, and the migration of hole carriers is more facilitated; the hole transport layer precursor solution is applied to the trans-perovskite battery, large-area lossless coating on the surface of the perovskite thin film can be realized, the performance and the stability of the prepared trans-perovskite battery are better, and the hole transport layer of the trans-perovskite solar battery is prepared in a large area by a sol-gel method, so that the trans-perovskite solar battery is easier to industrially produce.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
The invention provides a precursor solution of a hole transport layer, which comprises the following components: a hole transport material, a first diluent, and a second diluent;
according to some embodiments of the invention, the hole transport material is a compound of metallic nickel and/or a complex of metallic nickel, including but not limited to nickel (II) bis (2, 4-pentanedionate) hydrate, NiC2O4、NiSO4、NiSO4·7H2O、NiCO3、NiF2、NiBr2、NiI2、NiCl2·6H2O、NiCl2、Ni(OH)2、Ni(OH)3、Ni2O3、Ni(CO)4、(C2H5)2Ni、[Ni(NH3)6]Cl2、[Ni(CN)4]Cl2、Ni(NO3)2·H2O、[Ni(en)3]Cl2Or [ Ni (H) ]2O)6]Cl2At least one of; the molar concentration of the hole transport material can be 0.02-10 mol/L; specifically, the molar concentration of the hole transporting material may be 0.02mol/L, 0.1mol/L, 0.5mol/L, 0.7mol/L, 0.9mol/L, 1mol/L, 3mol/L, 5mol/L, 6mol/L, 7mol/L, 8mol/L, 9mol/L, 10mol/L, or the like;
according to some embodiments of the invention, the first diluent is selected from at least one of methanol, acetonitrile, water, chlorobenzene, toluene, ethanol, dimethylformamide, dimethyl sulfoxide, acetone, isopropanol, ethyl acetate, ammonia water or an aqueous methylamine solution; the first diluent is not capable of reacting with the hole transport material or/and the second diluent;
according to some embodiments of the invention, the second diluent is selected from at least one of ethanol, acetone, dioxane, tetrahydrofuran, methyl ethyl ketone, n-butanol, ethyl acetate, diethyl ether, isopropyl ether, dichloromethane, chloroform, bromoethane, benzene, carbon tetrachloride, carbon disulfide, cyclohexane, hexane; the hole transport material needs to be fully dissolved in the second diluent, if the hole transport material is not completely dissolved, a solid nickel metal compound or/and a nickel metal complex can be adhered to glass to cause protrusion, and the flatness of the film can be greatly reduced in the subsequent deposition of a functional film, so that the efficiency of the perovskite solar cell is reduced, and therefore stirring treatment needs to be carried out to completely dissolve the hole transport material;
according to some embodiments of the invention, the volume ratio of the first diluent to the second diluent may be 1: (0.1-1000); specifically, the volume ratio of the first diluent to the second diluent may be 1: 0.1, 1: 0.5, 1: 1. 1: 10. 1: 50. 1: 100. 1: 200. 1: 500. 1: 750. 1: 800. 1: 900. 1: 1000, etc.; if the amount of the second diluent is less than the above range, the hole transport material may not be completely dissolved; if the amount of the second diluent exceeds the above range, the precursor solution may be unevenly adhered to the glass.
Example 1
The embodiment provides a trans-perovskite solar cell and a preparation method thereof, and the preparation method comprises the following steps:
s1, cutting a 1cm multiplied by 1cm conductive glass substrate, and sequentially carrying out ultrasonic cleaning on the conductive glass substrate by an industrial cleaning agent, deionized water, ethanol and acetone until the surface has good wettability and no impurity residue; drying with compressed air, and treating in ultraviolet ozone machine for 30 min;
s2, placing the glass treated by the ultraviolet ozone on a heating table, and preheating at 400 ℃;
s3, preparing a hole transport layer precursor solution: the hole transport material is bis (2, 4-pentanedionate) nickel (II) hydrate, the first diluent is acetonitrile, the second diluent is ethanol, the molar concentration of the bis (2, 4-pentanedionate) nickel (II) hydrate is 0.03mol/L, and the volume ratio of the acetonitrile to the ethanol is 1: 50;
s4, loading the prepared hole transport layer precursor solution by using a spray gun, enabling the spray gun to be 40cm away from the substrate, horizontally spraying the hole transport layer precursor solution by the spray gun above the surface of the substrate in a zigzag manner, covering a heating cover after the coating is finished, carrying out heat treatment at 400 ℃ for 10min, setting the temperature to be 120 ℃, and removing excessive water in the film layer to obtain a uniform and compact hole transport layer;
s5, preparing the perovskite light absorption layer by spin coating, preparing a precursor solution according to the proportion of perovskite components, and weighing MAI and PbI according to the required stoichiometric ratio2The solvent is DMF: DMSO ═ 5: 1 (volume ratio), wherein the concentration of the precursor solution is 1.25mol/L, the spin-coating speed is 3000r/min, the spin-coating is carried out for 30s, and the prepared perovskite thin film is annealed for 5min at 105 ℃ on a heating table;
s6, preparing the electron transport layer on the perovskite light absorption layer by adopting a spin coating method, preparing 10mg/mL PCBM solution, carrying out spin coating at the speed of 5000r/min for 10S, and annealing the prepared electron transport layer on a heating table at the temperature of 75 ℃ for 5 min.
S7, manufacturing the metal electrode by adopting a vapor deposition method, adopting Ag as the electrode and having the thickness of 100 nm.
Example 2
The embodiment provides a trans-perovskite solar cell and a preparation method thereof, and the preparation method comprises the following steps:
s1, cutting a 1cm multiplied by 1cm conductive glass substrate, and sequentially carrying out ultrasonic cleaning on the conductive glass substrate by an industrial cleaning agent, deionized water, ethanol and acetone until the surface has good wettability and no impurity residue; drying with compressed air, and treating in ultraviolet ozone machine for 30 min;
s2, placing the glass treated by the ultraviolet ozone on a heating table, and preheating at 400 ℃;
s3, preparing a hole transport layer precursor solution: the hole transport material is Ni (OH)3The first diluent is methanol, the second diluent is ethyl acetate, Ni (OH)3Is at a molar concentration ofThe degree is 0.08mol/L, and the volume ratio of methanol to ethyl acetate is 1: 60, adding a solvent to the mixture;
s4, preparing the hole transport layer by adopting a spin coating method, wherein the spin coating speed is 1000r/min, the spin coating is carried out for 30S, and the prepared hole transport layer is annealed for 10min at 400 ℃ on a heating table;
s5, preparing the perovskite light absorption layer by spin coating, preparing a precursor solution according to the proportion of perovskite components, and weighing MAI and PbI according to the required stoichiometric ratio2The solvent is DMF: DMSO ═ 5: 1 (volume ratio), wherein the concentration of the precursor solution is 1.3mol/L, the spin-coating speed is 3000r/min, the spin-coating time is 30s, and the prepared perovskite thin film is annealed for 5min at 105 ℃ on a heating table;
s6, preparing the electron transport layer on the perovskite light absorption layer by adopting a spin coating method, preparing 10mg/mL PCBM solution, carrying out spin coating at the speed of 5000r/min for 10S, and annealing the prepared electron transport layer on a heating table at the temperature of 75 ℃ for 5 min.
S7, manufacturing the metal electrode by adopting a vapor deposition method, adopting Ag as the electrode and having the thickness of 100 nm.
Example 3
The embodiment provides a trans-perovskite solar cell and a preparation method thereof, and the preparation method comprises the following steps:
s1, cutting a 1cm multiplied by 1cm conductive glass substrate, and sequentially carrying out ultrasonic cleaning on the conductive glass substrate by an industrial cleaning agent, deionized water, ethanol and acetone until the surface has good wettability and no impurity residue; drying with compressed air, and treating in ultraviolet ozone machine for 30 min;
s2, placing the glass treated by the ultraviolet ozone on a heating table, and preheating at 400 ℃;
s3, preparing a hole transport layer precursor solution: the hole transport material is (C)2H5)2Ni, formamide as the first diluent, isopropyl ether as the second diluent, and (C)2H5)2The molar concentration of Ni is 0.12mol/L, and the volume ratio of formamide to isopropyl ether is 1: 14;
s4, preparing the hole transport layer by adopting a spin coating method, wherein the spin coating speed is 1500r/min, the spin coating is carried out for 30S, and the prepared hole transport layer is annealed for 10min at the temperature of 420 ℃ on a heating table;
s5, preparing the perovskite light absorption layer by spin coating, preparing a precursor solution according to the proportion of perovskite components, and weighing MAI and PbI according to the required stoichiometric ratio2The solvent is DMF: DMSO ═ 4: 1 (volume ratio), wherein the concentration of the precursor solution is 1.3mol/L, the spin-coating speed is 3000r/min, the spin-coating time is 30s, and the prepared perovskite thin film is annealed for 5min at 105 ℃ on a heating table;
s6, preparing the electron transport layer on the perovskite light absorption layer by adopting a spin coating method, preparing 10mg/mL PCBM solution, carrying out spin coating at the speed of 5000r/min for 10S, and annealing the prepared electron transport layer on a heating table at the temperature of 75 ℃ for 5 min.
S7, manufacturing the metal electrode by adopting a vapor deposition method, adopting Ag as the electrode and having the thickness of 100 nm.
Example 4
The embodiment provides a trans-perovskite solar cell and a preparation method thereof, and the preparation method comprises the following steps:
s1, cutting a 1cm multiplied by 1cm conductive glass substrate, and sequentially carrying out ultrasonic cleaning on the conductive glass substrate by an industrial cleaning agent, deionized water, ethanol and acetone until the surface has good wettability and no impurity residue; drying with compressed air, and treating in ultraviolet ozone machine for 30 min;
s2, placing the glass treated by the ultraviolet ozone on a heating table, and preheating at 400 ℃;
s3, preparing a hole transport layer precursor solution: the hole transport material is NiCO3The first diluent is water, the second diluent is dichloromethane or NiCO3Is 0.12mol/L, the volume ratio of water to dichloromethane is 1: 10;
s4, loading the prepared hole transport layer precursor solution by using a spray gun, enabling the spray gun to be 40cm away from the substrate, horizontally spraying the hole transport layer precursor solution by the spray gun above the surface of the substrate in a zigzag manner, covering a heating cover after the hole transport layer precursor solution is coated, carrying out heat treatment at 500 ℃ for 10min, setting the temperature to be 130 ℃, and removing excessive water in the film layer to obtain a uniform and compact hole transport layer;
s5, useThe preparation of perovskite light absorption layer is carried out on the hole transmission layer by spin coating method, precursor liquid is prepared according to the proportion of perovskite components, and MAI and PbI are weighed according to the required stoichiometric ratio2The solvent is DMF: DMSO ═ 4: 1 (volume ratio), wherein the concentration of the precursor solution is 1.3mol/L, the spin-coating speed is 3000r/min, the spin-coating time is 30s, and the prepared perovskite thin film is annealed for 5min at 105 ℃ on a heating table;
s6, preparing the electron transport layer on the perovskite light absorption layer by adopting a spin coating method, preparing 10mg/mL PCBM solution, carrying out spin coating at the speed of 5000r/min for 10S, and annealing the prepared electron transport layer on a heating table at the temperature of 75 ℃ for 5 min.
S7, manufacturing the metal electrode by adopting a vapor deposition method, adopting Ag as the electrode and having the thickness of 100 nm.
Comparative example
The present comparative example provides a trans-perovskite solar cell and a method of manufacturing the same, the steps of manufacturing comprising:
s1, cutting a 1cm multiplied by 1cm conductive glass substrate, and sequentially carrying out ultrasonic cleaning on the conductive glass substrate by an industrial cleaning agent, deionized water, ethanol and acetone until the surface has good wettability and no impurity residue; drying with compressed air, and treating in ultraviolet ozone machine for 30 min;
s2, preparing a hole transport layer precursor solution: the solute is Spiro-OMe TAD, the solvent is chlorobenzene, and the concentration of the Spiro-OMe TAD is 70 mg/mL;
s3, preparing the hole transport layer by adopting a spin coating method, wherein the spin coating speed is 5000r/min, and the spin coating time is 15S;
s4, preparing a perovskite light absorption layer on the hole transport layer by adopting a spin coating method, preparing a precursor solution according to the proportion of perovskite components, and weighing MAI and PbI according to the required stoichiometric ratio2The solvent is DMF: DMSO ═ 4: 1 (volume ratio), wherein the concentration of the precursor solution is 1.3mol/L, the spin-coating speed is 3000r/min, the spin-coating time is 30s, and the prepared perovskite thin film is annealed for 5min at 105 ℃ on a heating table;
s5, preparing the electron transport layer on the perovskite light absorption layer by adopting a spin coating method, preparing 10mg/mL PCBM solution, carrying out spin coating at the speed of 5000r/min for 10S, and annealing the prepared electron transport layer on a heating table at the temperature of 75 ℃ for 5 min.
S6, manufacturing the metal electrode by adopting a vapor deposition method, adopting Ag as the electrode and having the thickness of 100 nm.
Detection examples
Perovskite solar devices (effective area 0.09 cm) prepared according to examples 1-4 and comparative example2) The test was performed in an environment with a room temperature of 25 ℃ and a relative humidity of 30%, and the solar simulator was under a light intensity, and the data obtained were as follows:
TABLE 1
| JSC(mA/cm2) | Voc(mV) | FF(％) | PCE(％) | |
| Example 1 | 22.58 | 1103.5 | 81％ | 20.18 |
| Example 2 | 22.69 | 1195.6 | 82％ | 22.24 |
| Example 3 | 21.97 | 1136.4 | 78％ | 19.47 |
| Example 4 | 21.63 | 1165.3 | 80％ | 20.16 |
| Comparative example 1 | 18.73 | 963.2 | 70％ | 12.63 |
In conclusion, the hole transport layer precursor solution can be uniformly attached to the FTO glass by methods such as spraying and spin coating, and the NiOx hole transport layer with uniform coverage can be obtained after annealing, compared with other methods, NiOx crystals with better crystals can be obtained, and simultaneously, redundant water can be discharged at high temperature, so that the transmission of current carriers is facilitated, the transmission speed of the current carriers is improved, and the photoelectric conversion efficiency of the perovskite solar cell is improved; compared with NiOx prepared by using compounds to react with each other, the prepared NiOx has higher purity and is more beneficial to the migration of hole carriers because the hole transport layer precursor solution only contains a single nickel compound; the hole transport layer precursor solution is applied to the trans-perovskite battery, large-area lossless coating on the surface of the perovskite thin film can be realized, the performance and the stability of the prepared trans-perovskite battery are better, and the hole transport layer of the trans-perovskite solar battery is prepared in a large area by a sol-gel method, so that the trans-perovskite solar battery is easier to industrially produce.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example" or "some examples" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A hole transport layer precursor solution, comprising: a hole transport material, a first diluent, and a second diluent;
wherein the hole transport material is a compound of metallic nickel and/or a complex of metallic nickel, and the molar concentration of the hole transport material is 0.02-10 mol/L; the volume ratio of the first diluent to the second diluent is 1: (0.1-1000).
2. The hole transport layer precursor solution of claim 1, wherein the hole transport material is selected from the group consisting of nickel (II) hydrate bis (2, 4-pentanedionate), NiC2O4、NiSO4、NiSO4·7H2O、NiCO3、NiF2、NiBr2、NiI2、NiCl2·6H2O、NiCl2、Ni(OH)2、Ni(OH)3、Ni2O3、Ni(CO)4、(C2H5)2Ni、[Ni(NH3)6]Cl2、[Ni(CN)4]Cl2、Ni(NO3)2·H2O、[Ni(en)3]Cl2Or [ Ni (H) ]2O)6]Cl2At least one of (1).
3. The hole transport layer precursor solution according to claim 1, wherein the first diluent is at least one selected from methanol, acetonitrile, water, chlorobenzene, toluene, ethanol, dimethylformamide, dimethyl sulfoxide, acetone, isopropanol, ethyl acetate, ammonia water, and a methylamine water solution.
4. The hole transport layer precursor solution according to claim 1, wherein the second diluent is at least one selected from the group consisting of ethanol, acetone, dioxane, tetrahydrofuran, methyl ethyl ketone, n-butanol, ethyl acetate, diethyl ether, isopropyl ether, dichloromethane, chloroform, ethyl bromide, benzene, carbon tetrachloride, carbon disulfide, cyclohexane, and hexane.
5. A method for preparing a hole transport layer precursor solution according to any one of claims 1 to 4, comprising the steps of: and mixing the hole transport material, the first diluent and the second diluent, and performing dispersion treatment to obtain the hole transport layer precursor solution.
6. A hole transport layer prepared from the hole transport layer precursor solution according to any one of claims 1 to 4.
7. The hole transport layer according to claim 6, wherein the hole transport layer is prepared by at least one method selected from the group consisting of spin coating, spray coating, blade coating, dipping, and slit coating.
8. A trans-perovskite solar cell, comprising: an electrically conductive substrate, a hole transport layer, a perovskite light absorbing layer, an electron transport layer as claimed in any one of claims 6 to 7, a blocking layer and an electrode.
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