CN112490369A - Preparation method of semiconductor material, perovskite semiconductor device and preparation method thereof - Google Patents
Preparation method of semiconductor material, perovskite semiconductor device and preparation method thereof Download PDFInfo
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- CN112490369A CN112490369A CN202011292188.3A CN202011292188A CN112490369A CN 112490369 A CN112490369 A CN 112490369A CN 202011292188 A CN202011292188 A CN 202011292188A CN 112490369 A CN112490369 A CN 112490369A
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- organic amine
- carboxylate
- amine salt
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 58
- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000243 solution Substances 0.000 claims abstract description 49
- -1 tin carboxylate Chemical class 0.000 claims abstract description 44
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 42
- 239000000758 substrate Substances 0.000 claims abstract description 28
- 150000007942 carboxylates Chemical class 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 24
- 239000012266 salt solution Substances 0.000 claims abstract description 22
- 150000001409 amidines Chemical class 0.000 claims abstract description 19
- 238000000151 deposition Methods 0.000 claims abstract description 17
- 238000000137 annealing Methods 0.000 claims abstract description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 33
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- 238000004528 spin coating Methods 0.000 claims description 22
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 18
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 12
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 9
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- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052794 bromium Inorganic materials 0.000 claims description 9
- 229910052801 chlorine Inorganic materials 0.000 claims description 9
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
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- 238000000034 method Methods 0.000 claims description 6
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- 239000006229 carbon black Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
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- NITMACBPVVUGOJ-UHFFFAOYSA-N 2,2,2-trifluoroethanimidamide Chemical compound NC(=N)C(F)(F)F NITMACBPVVUGOJ-UHFFFAOYSA-N 0.000 claims description 4
- NJAHGEUFOYIGKR-UHFFFAOYSA-N 2-chloroethanimidamide Chemical compound NC(=N)CCl NJAHGEUFOYIGKR-UHFFFAOYSA-N 0.000 claims description 4
- WGTASENVNYJZBK-UHFFFAOYSA-N 3,4,5-trimethoxyamphetamine Chemical compound COC1=CC(CC(C)N)=CC(OC)=C1OC WGTASENVNYJZBK-UHFFFAOYSA-N 0.000 claims description 4
- OQLZINXFSUDMHM-UHFFFAOYSA-N Acetamidine Chemical compound CC(N)=N OQLZINXFSUDMHM-UHFFFAOYSA-N 0.000 claims description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 4
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 4
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 4
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 3
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- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 3
- 238000010248 power generation Methods 0.000 claims description 3
- UHOPWFKONJYLCF-UHFFFAOYSA-N 2-(2-sulfanylethyl)isoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(CCS)C(=O)C2=C1 UHOPWFKONJYLCF-UHFFFAOYSA-N 0.000 claims description 2
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 claims description 2
- LVZWSLJZHVFIQJ-UHFFFAOYSA-N Cyclopropane Chemical compound C1CC1 LVZWSLJZHVFIQJ-UHFFFAOYSA-N 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 230000023004 detection of visible light Effects 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 238000001548 drop coating Methods 0.000 claims description 2
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000007639 printing Methods 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 229940005605 valeric acid Drugs 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000002243 precursor Substances 0.000 abstract description 10
- 239000002798 polar solvent Substances 0.000 abstract description 9
- 239000007772 electrode material Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 239000010409 thin film Substances 0.000 description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 13
- 229940046892 lead acetate Drugs 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 10
- 229910052718 tin Inorganic materials 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 7
- 238000012876 topography Methods 0.000 description 7
- LLWRXQXPJMPHLR-UHFFFAOYSA-N methylazanium;iodide Chemical compound [I-].[NH3+]C LLWRXQXPJMPHLR-UHFFFAOYSA-N 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 description 4
- 239000012296 anti-solvent Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
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- 238000007790 scraping Methods 0.000 description 2
- ZMZDMBWJUHKJPS-UHFFFAOYSA-N thiocyanic acid Chemical compound SC#N ZMZDMBWJUHKJPS-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- ZVHAANQOQZVVFD-UHFFFAOYSA-N 5-methylhexan-1-ol Chemical compound CC(C)CCCCO ZVHAANQOQZVVFD-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- SBMMOLKBPGETHC-UHFFFAOYSA-N [I].NC=N Chemical compound [I].NC=N SBMMOLKBPGETHC-UHFFFAOYSA-N 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- ZFBGUXUJXUFOLU-UHFFFAOYSA-L butanoate;lead(2+) Chemical compound [Pb+2].CCCC([O-])=O.CCCC([O-])=O ZFBGUXUJXUFOLU-UHFFFAOYSA-L 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- NCBGOHTYKCLZMA-UHFFFAOYSA-J heptanoate tin(4+) Chemical compound [Sn+4].CCCCCCC([O-])=O.CCCCCCC([O-])=O.CCCCCCC([O-])=O.CCCCCCC([O-])=O NCBGOHTYKCLZMA-UHFFFAOYSA-J 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-M hexanoate Chemical compound CCCCCC([O-])=O FUZZWVXGSFPDMH-UHFFFAOYSA-M 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- FYDIWJWWROEQCB-UHFFFAOYSA-L lead(2+);propanoate Chemical compound [Pb+2].CCC([O-])=O.CCC([O-])=O FYDIWJWWROEQCB-UHFFFAOYSA-L 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- YZJQPSAZKVXWEZ-UHFFFAOYSA-J tin(4+) tetraformate Chemical compound [Sn+4].[O-]C=O.[O-]C=O.[O-]C=O.[O-]C=O YZJQPSAZKVXWEZ-UHFFFAOYSA-J 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- LSZKGNJKKQYFLR-UHFFFAOYSA-J tri(butanoyloxy)stannyl butanoate Chemical compound [Sn+4].CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O.CCCC([O-])=O LSZKGNJKKQYFLR-UHFFFAOYSA-J 0.000 description 1
- MFHJHZZHPOTAQY-UHFFFAOYSA-J tri(pentanoyloxy)stannyl pentanoate Chemical compound CCCCC(=O)O[Sn](OC(=O)CCCC)(OC(=O)CCCC)OC(=O)CCCC MFHJHZZHPOTAQY-UHFFFAOYSA-J 0.000 description 1
- LORRXSUXWWGUIX-UHFFFAOYSA-J tri(propanoyloxy)stannyl propanoate Chemical compound [Sn+4].CCC([O-])=O.CCC([O-])=O.CCC([O-])=O.CCC([O-])=O LORRXSUXWWGUIX-UHFFFAOYSA-J 0.000 description 1
- 229940070710 valerate Drugs 0.000 description 1
Images
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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
-
- 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
-
- 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
- H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
-
- 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
Abstract
The invention discloses a preparation method of a semiconductor material, a perovskite semiconductor device and a preparation method thereof, wherein the preparation method of the semiconductor material comprises the following steps: depositing a carboxylate solution, wherein the carboxylate solution is at least one selected from a lead carboxylate solution and a tin carboxylate solution; depositing an organic amine salt/amidine salt solution; annealing at 50-160 deg.c. The invention uses carboxylate and organic amine salt/amidine salt as raw materials, the used solvent can not contain strong polar and toxic solvents such as DMF, DMSO and the like, is suitable for growing perovskite on various substrates sensitive to polar solvents and insensitive to polar solvents, and is environment-friendly. The invention also utilizes carboxylate solution and organic amine salt/amidine salt solution as perovskite precursor material, and carries out crystallization in the carbon electrode, so that the carbon electrode material directly contacted with the perovskite layer is wrapped by the perovskite material, thereby increasing the contact area of the perovskite/carbon heterojunction and improving the photoelectric conversion performance and stability of the device.
Description
Technical Field
The invention relates to the technical field of semiconductor photoelectricity, in particular to a preparation method of a semiconductor material, a perovskite semiconductor device and a preparation method of the perovskite semiconductor device.
Background
The preparation method of the semiconductor material often determines the application range and the application field of the semiconductor material. The existing solution method for preparing the perovskite thin film requires that a substrate is insensitive to polar solvents, and toxic solvents such as DMF (dimethyl formamide), DMSO (dimethyl sulfoxide) and the like with strong polarity are used, so that adverse effects on the environment can be caused in future industrial production. For example, in the current anti-solvent method for preparing high-quality perovskite, most of solvents for dissolving perovskite precursor salt are DMF, DMSO belongs to strong polar solvents, and is not suitable for growing on a substrate sensitive to polar solvents. In addition, lead iodide is also used as the perovskite precursor salt in the prior art, and the lead iodide has good solubility only in strong polar solvents such as DMF, DMSO and the like, so that the use range of the substrate is limited, and the perovskite precursor salt is not environment-friendly and is not suitable for industrial production.
In order to further widen the application range of the perovskite semiconductor material and promote the further improvement of the performance of the related semiconductor device, a novel semiconductor preparation method needs to be developed.
The semiconductor device which can perform photoelectric conversion, photoelectric detection and photoelectric conversion is developed by utilizing the photoelectric property of the semiconductor, and the change of covering the ground is brought to social life. The halogen-containing perovskite semiconductor has the characteristics of excellent carrier mobility, high absorption coefficient and low-temperature solution preparation, so that the halogen-containing perovskite semiconductor has excellent performance and lower cost in the aspect of semiconductor devices. The carbon material has the advantages of low cost, high chemical stability, high temperature resistance and the like, the work function of the carbon material is matched with the valence band of the perovskite material, hole carriers in the perovskite material can be transferred, and carbon allotropes such as graphite, carbon black, graphene, carbon nanotubes and the like have good conductivity, so that the carbon film is used as an electrode in the perovskite solar cell and can collect holes and transmit the holes to an external circuit. In the prior art, a carbon electrode perovskite solar cell is prepared by directly coating carbon slurry on the surface of a perovskite film, good combination is formed between perovskite and the carbon slurry, and the cell has good long-term stability, but the defects of more interface defects and large interface resistance between a carbon electrode and a perovskite active layer exist, and the prepared solar cell has low efficiency and poor stability.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a preparation method of a semiconductor material, which can be suitable for various substrates sensitive or insensitive to polar solvents.
The invention also provides a preparation method of the perovskite semiconductor device, which can effectively improve the contact interface of the carbon electrode and the perovskite layer, and reduce the interface defect and the interface impedance, thereby greatly improving the efficiency of the perovskite solar cell and the stability of the device.
The invention also provides a perovskite semiconductor device.
The invention also provides application of the perovskite semiconductor device in power generation of the solar cell and detection of visible light signals.
In a first aspect of the present invention, there is provided a method of preparing a semiconductor material, comprising the steps of:
(1) depositing a carboxylate solution; or depositing organic amine salt or amidine salt solution and then depositing carboxylate salt solution; the carboxylate solution is at least one of lead carboxylate solution and tin carboxylate solution;
(2) depositing an organic amine salt or amidine salt solution;
annealing at 50-160 deg.c.
The preparation method of the semiconductor material provided by the embodiment of the invention has at least the following beneficial effects:
the embodiment of the invention uses carboxylate and organic amine salt as raw materials, and the used solvent can not contain strong polar and toxic solvents such as DMF, DMSO and the like, is suitable for growing perovskite on various substrates sensitive to polar solvents and insensitive to polar solvents, and is environment-friendly.
According to some embodiments of the invention, the organic amine salt or amidine salt in the organic amine salt solution has the formula AX, a is one or a combination of any two or a combination of three of methylamine, ethylamine, propylamine, butylamine, phenethylamine, ethylenediamine, propylenediamine, butylenediamine, pentylenediamine, formamidine, acetamidine, chloroacetamidine, and trifluoroacetamidine; b is lead and tin; x can be one of iodine, bromine and chlorine or a combination of any two or three of the iodine, the bromine and the chlorine.
According to some embodiments of the invention, the lead carboxylate has the formula Pb (C)nH2n-1OO)2N is 1 to 18, lead carboxylate is exemplified by lead formate, lead acetate, lead propionate, lead butyrate, lead valerate, and the formula of the tin carboxylate is Sn (C)nH2n- 1OO)2Examples of the tin carboxylate include tin formate, tin acetate, tin propionate, tin butyrate, tin valerate, tin caproate and tin heptanoate.
According to some embodiments of the invention, the solvent in the carboxylate solution is selected from at least one of acetic acid, propionic acid, butyric acid, valeric acid, isopropanol, propanol, tert-butanol, n-butanol, pentanol, tert-pentanol, ethyl acetate, ethyl formate, methyl acetate, propyl propionate.
According to some embodiments of the invention, the solvent in the organic amine salt or amidine salt solution is selected from at least one of methanol, ethanol, propanol, isopropanol, tert-butanol, cyclopropane, ethyl acetate.
According to some embodiments of the invention, the deposition in steps (1) and (2) is by at least one of spin coating, knife coating, slit coating, printing, drop coating, spray coating, roll-to-roll coating.
In a second aspect of the present invention, there is provided a method of manufacturing a perovskite semiconductor device, comprising the steps of:
sequentially preparing a substrate, a transparent conductive electrode, an electron transmission layer, a perovskite layer and a carbon electrode which are arranged in a stacked manner;
sequentially depositing a carboxylate solution and an organic amine salt or amidine salt solution on the carbon electrode, or sequentially depositing an organic amine salt or amidine salt solution, a carboxylate solution and an organic amine salt or amidine salt solution on the carbon electrode, wherein the carboxylate solution is selected from at least one of a lead carboxylate solution and a tin carboxylate solution, and the organic amine salt or amidine salt solution deposited for the first time and the organic amine salt or amidine salt solution deposited for the second time in the step can be the same or different;
annealing at 50-160 deg.c.
The preparation method of the perovskite semiconductor device provided by the embodiment of the invention has at least the following beneficial effects:
according to the embodiment of the invention, carboxylate solution and organic amine salt or amidine salt solution are used as perovskite precursor materials and are crystallized in the carbon electrode, so that the carbon electrode material directly contacted with the perovskite layer is wrapped by the perovskite material, the contact area of a perovskite/carbon heterojunction is increased, the interface charge transfer impedance is reduced, the carbon electrode charge collection efficiency is increased, and the photoelectric conversion performance and stability of the device are greatly improved. In addition, the perovskite precursor crystals can change the component distribution of the perovskite, and better interface energy level matching is formed.
The electron transport layer includes at least one of titanium oxide, zinc oxide, tin oxide, and graphene. The thickness of the electron transport layer is 5 to 500 nm. The transparent conductive electrode includes any one of ITO (indium tin oxide), FTO (fluorine doped tin oxide), AZO (aluminum doped zinc oxide).
According to some embodiments of the invention, the organic amine salt or amidine salt in the solution of the organic amine salt or amidine salt has the formula AX, a is one or a combination of any two or a combination of three of methylamine, ethylamine, propylamine, butylamine, phenethylamine, ethylenediamine, propylenediamine, butylenediamine, pentylenediamine, formamidine, acetamidine, chloroacetamidine, and trifluoroacetamidine; b is lead and tin; x can be one of iodine, bromine and chlorine or a combination of any two or three of the iodine, the bromine and the chlorine.
According to some embodiments of the invention, the carbon electrode is made of a mixture of materials including a carbon material, a binder, a dispersant and a solvent, preferably the carbon material includes at least one of graphite, carbon black, carbon nanotubes.
According to some embodiments of the invention, the perovskite in the perovskite layer is ABX3The perovskite type comprises at least one of Methylamine (MA), Formamidine (FA), cesium, rubidium, potassium and sodium, B comprises at least one of lead, tin, germanium, bismuth and titanium, and X comprises at least one of iodine, bromine, chlorine and thiocyanic acid.
In a third aspect of the present invention, there is provided a perovskite semiconductor device manufactured according to the above-described method for manufacturing a perovskite semiconductor device.
In a fourth aspect of the invention, the perovskite semiconductor device is applied to solar cell power generation and visible light signal detection.
Drawings
FIG. 1 is an electron microscope image of the surface morphology of the perovskite thin film prepared in example 1;
FIG. 2 is a surface topography of a perovskite substrate obtained in a conventional manner and a perovskite thin film obtained on the perovskite substrate in example 2;
FIG. 3 is an X-ray diffraction spectrum of the perovskite thin film obtained in example 6;
FIG. 4 is a graph comparing the J-V characteristics of the control device and the improved device of examples 7 and 8;
fig. 5 is a stability test chart of the perovskite semiconductor device in example 7.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and those skilled in the art can obtain other embodiments without inventive effort based on the embodiments of the present invention, and all embodiments are within the protection scope of the present invention.
Example 1
This embodiment provides a MAPbI3The preparation method of the perovskite semiconductor material comprises the following steps:
taking 60mg/mL lead acetate solution and acetic acid as a solvent, spin-coating 30 seconds on a common glass substrate at the rotating speed of 2000rpm, then spin-coating 30mg/mL MAI (methylamine hydroiodide) solution and isopropanol as a solvent, spin-coating 30 seconds at the rotating speed of 2000rpm, and heating at 100 ℃ for 10 minutes to obtain compact and smooth MAPbI3The surface micro-topography of the perovskite thin film is shown in FIG. 1.
Example 2
First, MAPbI prepared on a common glass substrate3Substrate: will PbI2And MAI was dissolved in DMSO and DMF at a volume ratio of 7:3 at a concentration of 1.47M, the anti-solvent was a mixture of toluene and ethyl acetate at a volume ratio of 7:3 at 1000rpm for 20s and 2000rpm for 50s, the anti-solvent was added dropwise over the last 10 seconds, followed by heating at 60 ℃ for 2 minutes and continuing heating at 100 ℃ for 5 minutes to obtain the perovskite substrate.
Preparing another layer of perovskite thin film on the obtained perovskite substrate: taking 15mg/mL MAI (methylamine hydroiodide) solution, taking isopropanol as solvent, carrying out spin coating for 30 seconds at the rotating speed of 2000rpm, then taking 18mg/mL lead acetate solution, taking acetic acid as solvent, carrying out spin coating for 30 seconds at the rotating speed of 2000rpm on the perovskite substrate, then carrying out spin coating for 15mg/mL MAI (methylamine hydroiodide) solution, taking isopropanol as solvent, carrying out spin coating for 30 seconds at the rotating speed of 2000rpm, and heating for 10 minutes at 100 ℃ to obtain the double-layer MAPbI3The surface micro-topography of the perovskite thin film is shown in fig. 2, wherein (a) represents a surface topography electron microscope image of the perovskite substrate, (b) represents a surface topography electron microscope image of the perovskite thin film prepared on the perovskite substrate, (c) represents a cross-sectional topography electron microscope image of the perovskite substrate in (a), and (d) represents a cross-sectional topography electron microscope image of the perovskite thin film prepared on the perovskite substrate in (b). As can be seen from the figure, the prepared double-layer perovskite thin film is smooth, has complete crystal grains, is integrated with the lower-layer perovskite thin film, and has better crystallinity.
Example 3
The embodiment provides an FA1-xMAxPbI3The preparation method of the perovskite semiconductor material comprises the following steps:
taking 18mg/mL lead acetate solution, taking a solvent as a mixture of acetic acid and ethanol, taking the ratio as 5 to 5, spin-coating on a PET substrate for 60 seconds at the rotating speed of 1000rpm, spin-coating 30mg/mL mixed solution of FAI (formamidine iodine) and MAI configured according to the stoichiometric ratio, taking the solvent as isopropanol, spin-coating for 60 seconds at the rotating speed of 1000rpm, and heating at 150 ℃ for 10 minutes to obtain FA1-xMAxPbI3A perovskite thin film.
Example 4
The embodiment provides an FA1-xMAxPb1-ySnyI3The preparation method of the perovskite semiconductor material comprises the following steps:
taking 6mg/mL mixed solution of lead acetate and tin acetate, taking a solvent which is a mixture of acetic acid and tert-butyl alcohol (the volume ratio is 1: 9), spin-coating on a common glass substrate for 60 seconds at the rotating speed of 1000rpm, spin-coating 9mg/mL mixed solution of FAI and MAI which are configured according to the stoichiometric ratio, taking the solvent which is isopropanol, spin-coating for 60 seconds at the rotating speed of 1000rpm, and heating at 100 ℃ for 10 minutes to obtain FA1-xMAxPb1-ySnyI3A perovskite thin film.
Example 5
This embodiment provides a MAPbI3The preparation method of the perovskite semiconductor material comprises the following steps:
taking 400mg/mL lead acetate solution, taking acetic acid as solvent, and dissolving in FTO/TiO2Spin-coating on the substrate at 2000rpm for 60 s, spin-coating 50mg/mL MAI solution with the solvent of ethanol and isopropanol at 800rpm for 60 s, and heating at 100 deg.C for 30min to obtain MAPbI3A perovskite thin film.
Example 6
This embodiment provides a MAPbI3The preparation method of the perovskite semiconductor material comprises the following steps:
dripping 15mg/mL MAI isopropanol solution on FTO/TiO2Drying the substrate, and dripping 18mg/mL lead acetate solution on FTO/TiO2On the MAI substrate, after 8 minutes, 12mg/mL MAI isopropanol solution is dripped on FTO/TiO2Heating for 5 minutes on a/MAI/lead acetate substrate at 100 ℃ for 30 minutes to obtain FTO/TiO2/MAPbI3The XRD pattern of the perovskite thin film is shown in figure 3, and the result shows that the characteristic diffraction peak of the (110) crystal face of the perovskite is sharp and the crystal phase is relatively pure.
Example 7
The embodiment provides a preparation method of a perovskite semiconductor device, which comprises the following steps:
(1) spin-coating a mesoporous layer TiO with the thickness of 300nm on an FTO glass substrate2Then in a one-step processSpin coating MAPbI3And (3) dripping a mixed solvent of toluene and ethyl acetate into the precursor solution 10s before the spin coating is finished, and annealing at 100 ℃ for 15min to obtain a compact perovskite layer. Graphite, carbon black, polymethyl methacrylate and isoheptanol are taken to form carbon slurry, and the carbon slurry is coated on the prepared perovskite layer as a carbon electrode in a scraping way to form a basic semiconductor device.
(2) Taking 6mg/mL lead acetate solution, the solvent is mixed solvent of acetic acid and ethanol, dripping on the surface of a carbon electrode of a basic semiconductor device, standing for 8 minutes, then dripping 12mg/mL MAI (methylamine hydroiodide) isopropanol solution, and then placing on a 100 ℃ hot bench for heating and annealing to form the perovskite semiconductor device.
In the embodiment, the perovskite precursor material lead acetate solution and methylamine hydroiodide are dropwise coated on the carbon electrode, so that the lead acetate solution and methylamine hydroiodide permeate into the carbon electrode and are crystallized in the carbon electrode, the carbon electrode material directly contacted with the perovskite layer is wrapped by the perovskite material, the contact area of the perovskite/carbon heterojunction is increased, the interface charge transfer impedance is reduced, the carbon electrode charge collection efficiency is increased, and the photoelectric conversion performance and stability of the device are greatly improved.
Taking the basic semiconductor device prepared in the step (1) as a solar cell for testing, wherein the photoelectric conversion efficiency is 11.3%, the open-circuit voltage is 0.952V, and the short-circuit current density is 19.87mA/cm2The fill factor was 60%, as shown in fig. 4 for control device 1. The perovskite semiconductor device obtained after the treatment of the step (2) is used as a solar cell for testing, the photoelectric conversion efficiency is 15.2%, the open-circuit voltage is 0.993V, and the short-circuit current density is 20.17mA/cm2The fill factor is 76%, as shown in the improved device 1 in fig. 4, experimental results show that perovskite grows in the carbon electrode, the interface contact resistance of the carbon electrode and the perovskite layer is improved, and further the photoelectric performance of the device is improved.
The stability of the perovskite semiconductor device prepared in the embodiment in the air under the non-packaging condition is measured, and the result is shown in fig. 5, after 2000 hours, the photoelectric conversion efficiency of the non-packaged device is not obviously attenuated, which indicates that the stability of the device obtained after filling the perovskite with the carbon electrode is also greatly improved.
Example 8
The embodiment provides a preparation method of a perovskite semiconductor device, which comprises the following steps:
(1) spin-coating a mesoporous layer TiO with the thickness of 300nm on an FTO glass substrate2Then using one-step spin coating MAPbI3And (3) dripping a toluene solvent into the precursor solution 10s before the spin coating is finished, and annealing at 100 ℃ for 30min to obtain a compact perovskite layer. Graphite, carbon black, polymethyl methacrylate and isopropanol are taken to be compounded to form carbon slurry, and the prepared perovskite layer is coated with the carbon slurry as a carbon electrode in a scraping way to form the basic semiconductor device.
(2) And (3) dropwise coating 15mg/mL of FAI/MAI isopropanol solution on the surface of a carbon electrode of a basic semiconductor device for 8 minutes, then dropwise coating a mixed solution of tin acetate and lead acetate, drying, then dropwise coating 30mg/mL of FAI/MAI isopropanol solution, standing for 8 minutes, and then placing on a 100 ℃ hot table for heating and annealing to form the perovskite semiconductor device.
In this embodiment, the perovskite precursor solution is infiltrated into the carbon electrode in a manner of sequentially depositing an organic amine salt/amidine salt, tin acetate/lead acetate, and an organic amine salt/amidine salt, so that the perovskite formed after annealing grows in the carbon electrode.
Taking the base semiconductor device prepared in the step (1) as a solar cell for testing, wherein the testing result is shown in a comparison device 2 in a graph 4, the photoelectric conversion efficiency is 10.8%, the open-circuit voltage is 0.947V, and the short-circuit current density is 19.69mA/cm2The fill factor is 58%. The perovskite semiconductor device obtained after the treatment in the step (2) is used as a solar cell for testing, and the test result is shown in an improved device 2 in fig. 4, wherein the photoelectric conversion efficiency is 15.5%, the open-circuit voltage is 1.004V, and the short-circuit current density is 20.27mA/cm2And the filling factor is 76%, which shows that the perovskite grows in the carbon electrode, the interface contact resistance of the carbon electrode and the perovskite layer is improved, and the photoelectric property of the device is further improved.
Claims (10)
1. The preparation method of the semiconductor material is characterized by comprising the following steps:
(1) depositing a carboxylate solution; or depositing organic amine salt or amidine salt solution and then depositing carboxylate salt solution; the carboxylate solution is at least one of lead carboxylate solution and tin carboxylate solution;
(2) depositing an organic amine salt or amidine salt solution;
(3) annealing at 50-160 deg.c.
2. The preparation method of claim 1, wherein the formula of the organic amine salt or amidine salt in the organic amine salt or amidine salt solution is AX, A is one or a combination of any two or a combination of three of methylamine, ethylamine, propylamine, butylamine, phenethylamine, ethylenediamine, propylenediamine, butylenediamine, pentylenediamine, formamidine, acetamidine, chloroacetamidine and trifluoroacetamidine; b is lead and tin; x can be one of iodine, bromine and chlorine or a combination of any two or three of the iodine, the bromine and the chlorine.
3. The method according to claim 1, wherein the solvent in the carboxylate solution is at least one selected from the group consisting of acetic acid, propionic acid, butyric acid, valeric acid, isopropyl alcohol, propyl alcohol, t-butyl alcohol, n-butyl alcohol, amyl alcohol, t-amyl alcohol, ethyl acetate, ethyl formate, methyl acetate, and propyl propionate.
4. The method according to claim 1, wherein the solvent in the organic amine salt or amidine salt solution is at least one selected from methanol, ethanol, propanol, isopropanol, tert-butanol, cyclopropane, and ethyl acetate.
5. The production method according to any one of claims 1 to 4, wherein the manner of deposition in steps (1) and (2) is at least one of spin coating, blade coating, slit coating, printing, drop coating, spray coating, and roll-to-roll coating.
6. The preparation method of the perovskite semiconductor device is characterized by comprising the following steps:
sequentially preparing a substrate, a transparent conductive electrode, an electron transmission layer, a perovskite layer and a carbon electrode which are arranged in a stacked manner;
sequentially depositing a carboxylate solution and an organic amine salt or amidine salt solution on the carbon electrode, or sequentially depositing an organic amine salt or amidine salt solution, a carboxylate solution, and an organic amine salt or amidine salt solution on the carbon electrode, wherein the carboxylate solution is selected from at least one of a lead carboxylate solution and a tin carboxylate solution;
annealing at 50-160 deg.c.
7. The method for producing a perovskite semiconductor device according to claim 6, wherein the formula of the organic amine salt or amidine salt in the organic amine salt or amidine salt solution is AX, A is one or a combination of any two or a combination of three of methylamine, ethylamine, propylamine, butylamine, phenethylamine, ethylenediamine, propylenediamine, butylenediamine, pentylenediamine, formamidine, acetamidine, chloroacetamidine, and trifluoroacetamidine; b is lead and tin; x can be one of iodine, bromine and chlorine or a combination of any two or three of the iodine, the bromine and the chlorine.
8. The method for producing a perovskite semiconductor device as claimed in claim 6, wherein the carbon electrode is made by mixing materials including a carbon material, a binder, a dispersant and a solvent, preferably wherein the carbon material includes at least one of graphite, carbon black, carbon nanotubes.
9. A perovskite semiconductor device characterized by being produced by the production method for a perovskite semiconductor device according to any one of claims 6 to 8.
10. Use of the perovskite semiconductor device according to claim 9 for power generation in solar cells, for detection of visible light signals.
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