CN115322216B - Lithium salt solvent for preparing organic-inorganic hybrid titanium ore solar battery - Google Patents
Lithium salt solvent for preparing organic-inorganic hybrid titanium ore solar battery Download PDFInfo
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- CN115322216B CN115322216B CN202210502823.9A CN202210502823A CN115322216B CN 115322216 B CN115322216 B CN 115322216B CN 202210502823 A CN202210502823 A CN 202210502823A CN 115322216 B CN115322216 B CN 115322216B
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 239000010936 titanium Substances 0.000 title claims abstract description 16
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 16
- 239000002904 solvent Substances 0.000 title abstract description 10
- 229910003002 lithium salt Inorganic materials 0.000 title abstract description 6
- 159000000002 lithium salts Chemical class 0.000 title abstract description 6
- 230000005525 hole transport Effects 0.000 claims abstract description 13
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims abstract description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 18
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 12
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000004528 spin coating Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 230000031700 light absorption Effects 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 5
- -1 amine salt Chemical class 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- JKSIBASBWOCEBD-UHFFFAOYSA-N N,N-bis(4-methoxyphenyl)-9,9'-spirobi[fluorene]-1-amine Chemical compound COc1ccc(cc1)N(c1ccc(OC)cc1)c1cccc2-c3ccccc3C3(c4ccccc4-c4ccccc34)c12 JKSIBASBWOCEBD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000002207 thermal evaporation Methods 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 230000005012 migration Effects 0.000 abstract description 7
- 238000013508 migration Methods 0.000 abstract description 7
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 6
- 239000010409 thin film Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 230000006798 recombination Effects 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 3
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 239000010408 film Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention belongs to the technical field of solar cells, and particularly relates to a lithium salt solvent for preparing an organic-inorganic hybrid titanium ore solar cell. In order to solve the problems of device failure and the like caused by migration of Li ions in a hole transport layer, the invention takes mercaptopropyl trimethoxysilane as a novel Li salt solvent, which not only can effectively inhibit migration of Li ions, but also can effectively reduce defects of perovskite thin films, reduce interface non-radiative recombination of devices, and finally improve the efficiency and stability of the devices obviously, thereby promoting commercialization and large-scale progress of perovskite solar cells.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a lithium salt solvent for preparing an organic-inorganic hybrid titanium ore solar cell.
Background
According to statistics, hydrogen energy, wind energy, nuclear energy, solar energy and the like are developed. Among them, solar energy is regarded as an inexhaustible clean energy source. So far, solar cells have come to third generation thin film solar cells. It is worth mentioning that since 2012 perovskite materials have been considered as non-two options for solar cells due to their excellent absorption coefficient, suitable band gap, high tolerance factor, etc. At present, the efficiency of perovskite solar cells has broken through 25.5%, which is comparable to silicon cells. However, there are still some problems that need to be addressed, such as film defects, non-radiative recombination at the interface, and ion migration between functional layers.
Lithium bistrifluoromethane sulfonimide (Li salt) used in the hole transport layer has been widely demonstrated to facilitate hole transport in the hole transport layer. However, migration of Li ions accelerates the failure of the device. This is because Li ions chemically react with halogen in perovskite during migration, thereby deteriorating the stability of the thin film. Therefore, how to suppress lithium ion migration in the hole transport layer is critical to the commercialization process of perovskite solar cells.
Disclosure of Invention
The present invention has been made in view of the above problems, and provides a lithium salt solvent for preparing an organic-inorganic hybrid titanium solar cell.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a lithium salt solvent for preparing organic-inorganic hybrid titanium ore solar cells is mercaptopropyl trimethoxysilane.
Further, the preparation method of the organic-inorganic hybrid titanium ore solar cell comprises the following steps:
step 1, conducting glass is subjected to ultrasonic treatment by sequentially using a detergent, deionized water and absolute ethyl alcohol, then dried, treated by ultraviolet ozone and taken out for standby;
step 2, mixing distilled water and titanium tetrachloride, soaking the conductive glass subjected to ozone treatment in the step 1 in the mixed solution, drying, taking out, flushing with distilled water, drying with nitrogen, annealing to obtain an electron transport layer, and then carrying out ultraviolet ozone treatment on the electron transport layer;
step 3, dissolving the perovskite light absorption layer material in a mixed solvent of DMF and DMSO to obtain a perovskite precursor solution, oscillating, filtering, spin-coating on an electron transmission layer, and then annealing, wherein chlorobenzene is dropwise added before spin-coating of the perovskite precursor solution is finished;
step 4, dissolving a hole transport layer material in chlorobenzene, adding a mercaptopropyl trimethoxysilane solution of TBP and Li-TFSI, uniformly mixing, and spin-coating onto the perovskite light absorption layer prepared in the step 3 to prepare a hole transport layer;
and 5, evaporating a metal back electrode on the hole transport layer prepared in the step 4 by thermal evaporation under high vacuum.
Further, in the step 1, the conductive glass is ITO or FTO, the ultrasonic treatment time is 20min, and the ultraviolet ozone treatment time is 20-30 min.
Further, in the step 2, the volume ratio of distilled water to titanium tetrachloride is 1:1-3, the drying temperature is 75 ℃, the time is 45min, the annealing temperature is 200 ℃, the time is 30min, and the ultraviolet ozone treatment time is 20-30 min.
Further, in the step 3, the perovskite light absorption layer material is organic amine salt and lead halide salt, and the volume ratio of DMF to DMSO is 4:1.
Further, in the step 3, the time of the shaking is 5min, the speed of the spin coating is 4000rpm, the time is 30s, the temperature of the annealing is 130 ℃ and the time is 28min.
Further, the hollow transmission layer material in the step 4 is 2,2', 7' -tetra [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spirobifluorene.
Further, the concentration of the mercaptopropyl trimethoxysilane solution of Li-TFSI in the step 4 is 250-520 mg/mL.
Further, the spin coating in the step 4 has a speed of 3000rpm for 30s.
Further, in the step 5, the metal back electrode is gold, silver, copper or aluminum, and the evaporation thickness is 100nm.
Compared with the prior art, the invention has the following advantages:
the Li salt is dissolved in mercaptopropyl trimethoxysilane to replace the acetonitrile solvent commonly used at present. By using mercaptopropyl trimethoxysilane, li ion migration in the hole transport layer is significantly suppressed. Meanwhile, the defects of the perovskite film are effectively reduced, and the average service life of the film is obviously prolonged. In addition, the interface non-radiative recombination of the device is also significantly suppressed. This contributes to an improvement in device performance. At the same time, the moderate stability of the device is also significantly improved, which promotes the commercialization process of perovskite solar cells.
Drawings
FIG. 1 is a current-voltage sweep graph of the perovskite solar cell of comparative example and example 1;
fig. 2 is a carrier lifetime graph of perovskite solar cells in comparative examples and example 1;
FIG. 3 is a current-voltage sweep graph of the perovskite solar cell of example 2;
fig. 4 is a current-voltage sweep graph of the perovskite solar cell of example 3.
Detailed Description
Comparative example
The preparation method of the organic-inorganic hybrid titanium ore solar cell comprises the following steps:
(1) Sequentially carrying out ultrasonic treatment on an FTO conductive substrate by using a detergent, deionized water and absolute ethyl alcohol for 20min, drying by blow-drying, then carrying out ultraviolet ozone treatment for 30min, and taking out for later use;
(2) Distilled water and titanium tetrachloride were mixed in an amount of 1:2.25, soaking the FTO in the step (1) in the mixed solution, placing the soaked FTO in an oven at 75 ℃ for 45 minutes, taking out the FTO, flushing the FTO with distilled water for several times, drying the FTO with nitrogen, annealing the dried FTO on a hot table at 200 ℃ for 30 minutes to obtain an electron transport layer, and carrying out ultraviolet ozone irradiation treatment on the electron transport layer for 20 minutes;
(3) FAI (248 mg), pbBr 2 (8.5mg)、RbI(6.6mg)、MACl(35.0mg)、PbI 2 (682.7 mg), csI (19.7 mg) and PbCl 2 (12.7 mg) was dissolved in a mixture of DMF and DMSO (V DMF :V DMSO After shaking for 5min, =4:1), the perovskite solution was dropped onto the electron transport layer prepared in step (2), spin-coated at 4000rpm for 30s, followed by annealing at 130 ℃ for 28min, wherein 80 μl of chlorobenzene was dropped within 2s 16s before the spin-coating of the perovskite solution was completed, to prepare a perovskite light absorption layer;
(4) 72.3mg of 2,2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene (Spiro-OMeTAD) was dissolved in lmL chlorobenzene, 29. Mu.L of TBP and 18. Mu.L of Li-TFSI (concentration: 520mg/mL, solvent: anhydrous acetonitrile) were added, and after mixing, the mixture was dropped onto the perovskite light absorbing layer obtained in the step (3), and spin-coated at a speed of 3000rpm for 30s, to obtain a hole transporting layer;
(5) In a high vacuum (10) -4 Pa), evaporating an Ag electrode with a thickness of 80nm on the hole transport layer prepared in step (4) by thermal evaporation.
Example 1
The difference from the comparative example is that in step (4), li-TFSI is mercaptopropyl trimethoxysilane as the solvent at a concentration of 520mg/mL.
Fig. 1 is a current-voltage sweep graph of the perovskite solar cell in comparative example and example 1, and it can be seen from fig. 1 that the efficiency of the perovskite solar cell in example 1 is significantly improved.
Fig. 2 is a carrier lifetime graph of the perovskite solar cell in comparative example and example 1, and it is known that carrier extraction of the perovskite thin film in example 1 is significantly improved.
Example 2
The difference from example 1 is that the concentration of Li-TFSI was changed to 250mg/mL.
Fig. 3 is a current-voltage plot of the perovskite solar cell of example 2 showing a 21.52% efficiency improvement in device efficiency compared to the cell of the comparative example (20.73%).
Example 3
The difference from example 1 is that the concentration of Li-TFSI was changed to 350mg/mL.
Fig. 4 is a current-voltage plot of the perovskite solar cell of example 3 showing a 21.85% efficiency improvement in device efficiency compared to the cell of the comparative example (20.73%).
Claims (9)
1. The preparation method of the organic-inorganic hybrid titanium ore solar cell is characterized by comprising the following steps of:
step 1, conducting glass is subjected to ultrasonic treatment by sequentially using a detergent, deionized water and absolute ethyl alcohol, then dried, treated by ultraviolet ozone and taken out for standby;
step 2, mixing distilled water and titanium tetrachloride, soaking the conductive glass subjected to ozone treatment in the step 1 in the mixed solution, drying, taking out, flushing with distilled water, drying with nitrogen, annealing to obtain an electron transport layer, and then carrying out ultraviolet ozone treatment on the electron transport layer;
step 3, dissolving the perovskite light absorption layer material in a mixed solvent of DMF and DMSO to obtain a perovskite precursor solution, oscillating, filtering, spin-coating on an electron transmission layer, and then annealing, wherein chlorobenzene is dropwise added before spin-coating of the perovskite precursor solution is finished;
step 4, dissolving a hole transport layer material in chlorobenzene, adding a mercaptopropyl trimethoxysilane solution of TBP and Li-TFSI, uniformly mixing, and spin-coating onto the perovskite light absorption layer prepared in the step 3 to prepare a hole transport layer;
and 5, evaporating a metal back electrode on the hole transport layer prepared in the step 4 by a thermal evaporation method under high vacuum.
2. The method for preparing the organic-inorganic hybrid titanium ore solar cell according to claim 1, wherein the conductive glass in the step 1 is ITO or FTO, the ultrasonic treatment time is 20min, and the ultraviolet ozone treatment time is 20-30 min.
3. The method for preparing the organic-inorganic hybrid titanium ore solar cell according to claim 1, wherein the volume ratio of distilled water to titanium tetrachloride in the step 2 is 1:1-3, the drying temperature is 75 ℃, the time is 45min, the annealing temperature is 200 ℃, the time is 30min, and the ultraviolet ozone treatment time is 20-30 min.
4. The method for preparing the organic-inorganic hybrid titanium ore solar cell according to claim 1, wherein the perovskite light absorbing layer material in the step 3 is organic amine salt and lead halide salt, and the volume ratio of DMF to DMSO is 4:1.
5. The method for preparing an organic-inorganic hybrid titanium ore solar cell according to claim 1, wherein the time of the shaking in the step 3 is 5min, the spin coating speed is 4000rpm, the time is 30s, the annealing temperature is 130 ℃, and the time is 28min.
6. The method for preparing an organic-inorganic hybrid titanium ore solar cell according to claim 1, wherein the hollow transmission layer material in the step 4 is 2,2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene.
7. The method for preparing the organic-inorganic hybrid titanium ore solar cell according to claim 1, wherein the concentration of the mercaptopropyl trimethoxysilane solution of Li-TFSI in the step 4 is 250-520 mg/mL.
8. The method for preparing an organic-inorganic hybrid titanium solar cell according to claim 1, wherein the spin-coating speed in the step 4 is 3000rpm for 30s.
9. The method for preparing an organic-inorganic hybrid titanium-ore solar cell according to claim 1, wherein the metal back electrode in the step 5 is gold, silver, copper or aluminum, and the evaporation thickness is 100nm.
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CN114400291A (en) * | 2022-01-18 | 2022-04-26 | 山西大学 | Application of organic molecules in positive perovskite solar cell |
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- 2022-05-09 CN CN202210502823.9A patent/CN115322216B/en active Active
Patent Citations (7)
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CN1771304A (en) * | 2003-04-10 | 2006-05-10 | 帝斯曼知识产权资产管理有限公司 | Curable liquid composition, cured film, and antistatic laminate |
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CN1922267A (en) * | 2004-03-22 | 2007-02-28 | 捷时雅股份有限公司 | Curable liquid resin composition and method for producing multilayer body using same |
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