CN115537973B - Molybdenum sulfide/porous carbon nanofiber composite electrode material and preparation method and application thereof - Google Patents
Molybdenum sulfide/porous carbon nanofiber composite electrode material and preparation method and application thereof Download PDFInfo
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- CN115537973B CN115537973B CN202211184632.9A CN202211184632A CN115537973B CN 115537973 B CN115537973 B CN 115537973B CN 202211184632 A CN202211184632 A CN 202211184632A CN 115537973 B CN115537973 B CN 115537973B
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- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000007772 electrode material Substances 0.000 title claims abstract description 51
- 239000002133 porous carbon nanofiber Substances 0.000 title claims abstract description 49
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 42
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 14
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000010000 carbonizing Methods 0.000 claims abstract description 8
- 150000002751 molybdenum Chemical class 0.000 claims abstract description 4
- 238000000137 annealing Methods 0.000 claims description 36
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 34
- 239000011521 glass Substances 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 238000004528 spin coating Methods 0.000 claims description 20
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 19
- JAHFQMBRFYOPNR-UHFFFAOYSA-N iodomethanamine Chemical compound NCI JAHFQMBRFYOPNR-UHFFFAOYSA-N 0.000 claims description 19
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 239000004408 titanium dioxide Substances 0.000 claims description 16
- 238000010521 absorption reaction Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 239000011888 foil Substances 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 7
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 7
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical group [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 7
- 229940116411 terpineol Drugs 0.000 claims description 7
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 7
- 238000007639 printing Methods 0.000 claims description 5
- 238000007790 scraping Methods 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000001523 electrospinning Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000011161 development Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 24
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 13
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 238000005530 etching Methods 0.000 description 11
- 229920000049 Carbon (fiber) Polymers 0.000 description 9
- 239000004917 carbon fiber Substances 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000005303 weighing Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000377 silicon dioxide Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 229920000742 Cotton Polymers 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 4
- 239000002134 carbon nanofiber Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000003599 detergent Substances 0.000 description 4
- 238000007598 dipping method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000003892 spreading Methods 0.000 description 4
- 230000007480 spreading Effects 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000005525 hole transport Effects 0.000 description 2
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000007547 defect 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
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal sulfide Chemical class 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention relates to the technical field of solar cells, and particularly discloses a molybdenum sulfide/porous carbon nanofiber composite electrode material, a preparation method and application thereof. The preparation method comprises the following steps: adding polyacrylonitrile and soluble molybdenum salt into N, N-dimethylformamide, and uniformly mixing to obtain spinning solution; carrying out electrostatic spinning on the spinning solution to obtain a spinning film; calcining the spinning film at 200-250 ℃ for 1-3 h, and carbonizing at 800-1000 ℃ for 1-3 h under inert atmosphere to obtain the molybdenum sulfide/porous carbon nanofiber composite electrode material. The perovskite solar cell prepared by the method has the advantages of high efficiency, stability and low cost, and the development of the preparation technology provides a new device preparation strategy for the commercialized application of the large-area perovskite solar cell.
Description
Technical Field
The invention relates to the technical field of solar cells, in particular to a molybdenum sulfide/porous carbon nanofiber composite electrode material, and a preparation method and application thereof.
Background
In recent years, perovskite as a photosensitive material has been attracting attention from research and development personnel because of its unique photoelectric effect, such as high absorption coefficient and carrier mobility, adjustable band gap, long carrier diffusion length, and significant tolerance to defects. The power conversion efficiency of perovskite solar cells has been improved to over 25% at present, which is comparable to commercial silicon-based solar cells. So far, it has been studied how to improve the performance of small-area perovskite solar cells, while large-area perovskite solar cells have been studied less due to their lower photoelectric conversion efficiency and higher material cost. Therefore, how to manufacture a high-efficiency and low-cost large-area perovskite solar cell is a key problem that must be solved to realize commercial applications of perovskite solar cells.
Carbon fiber is used as a functional carbon material with good conductivity, has good hydrophobicity and is often used as an electrode material, and although the contact area between a back electrode taking carbon fiber as a main material and a perovskite absorption layer is relatively large, the carbon fiber is still insufficient to effectively improve the efficiency of a carbon-based perovskite solar cell, so that the large-scale application of the perovskite solar cell is limited. Therefore, a novel functional carbon material is developed to improve the stability and the photoelectric conversion efficiency of the large-area perovskite solar cell, and has great significance for promoting the commercialized application of the large-area perovskite solar cell.
Disclosure of Invention
Aiming at the problem of low photoelectric conversion efficiency when the existing carbon-based functional material is applied to a perovskite solar cell, the invention provides a molybdenum sulfide/porous carbon nanofiber composite electrode material, and a preparation method and application thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
A preparation method of a molybdenum sulfide/porous carbon nanofiber composite electrode material comprises the following steps:
Step a, adding polyacrylonitrile and soluble molybdenum salt into N, N-dimethylformamide, and uniformly mixing to obtain spinning solution;
Step b, carrying out electrostatic spinning on the spinning solution to obtain a spinning film;
and c, calcining the spinning film at 200-250 ℃ for 1-3 h, and carbonizing at 800-1000 ℃ for 1-3 h in an inert atmosphere to obtain the molybdenum sulfide/porous carbon nanofiber composite electrode material.
For the prior art, the preparation method of the molybdenum sulfide/porous carbon nanofiber composite electrode material provided by the invention has the advantages that the prepared molybdenum sulfide/porous carbon nanofiber composite electrode material has a multi-stage network porous structure, the specific surface area of the composite material is obviously increased, the interface contact of a perovskite absorption layer is improved, and the improvement of the filling factor of a perovskite solar cell is facilitated; meanwhile, molybdenum sulfide doped in the carbon fiber is layered transition metal sulfide similar to graphite in structure, strong covalent bond combination is formed in the molybdenum sulfide layer, and weak van der Waals force connection is formed between the layers, so that the composite electrode material has better ion conductivity, carrier recombination at an interface is reduced, and the open-circuit voltage of the perovskite solar cell is improved; in addition, molybdenum sulfide is adopted to dope the carbon fiber, so that the energy level of the carbon fiber can be effectively regulated and controlled, the matching degree between the carbon fiber and the perovskite energy level is higher, the transmission of holes in the perovskite solar cell is facilitated, and the hole transmission efficiency is increased; the molybdenum sulfide/porous carbon nanofiber composite electrode material is prepared into a back electrode, can also serve as a hole transport layer, improves carrier mobility, improves overall battery efficiency, and has wide application prospects in the field of perovskite solar cells.
Preferably, in step a, the soluble molybdate is ammonium tetrathiomolybdate.
Preferably, in the step a, the mass ratio of the polyacrylonitrile to the soluble molybdate is 4-6:1.
Preferably, in the step a, the mass concentration of the polyacrylonitrile in the spinning solution is 8% -15%.
The addition of the polyacrylonitrile and the soluble molybdate can enable the back electrode prepared from the prepared molybdenum sulfide/porous carbon nanofiber composite material to have a proper work function, so that the separation efficiency of electrons and holes is improved, and the photoelectric conversion efficiency of the perovskite solar cell is improved obviously.
Preferably, in the step b, the parameters of the electrospinning are as follows: the loading voltage is 15kV-20kV, the distance between the spray head and the aluminum foil is 15cm-20cm, the flow rate is 1mL/h-1.5mL/h, and the humidity is 25% -35%.
The preferred parameters of electrospinning are advantageous for obtaining a continuous nanofiber membrane.
Further, in the step b, the parameters of the electrospinning are as follows: the loading voltage is 18kV, the distance between the spray head and the aluminum foil is 15cm, the flow rate is 1.2mL/h, and the humidity is 30%.
Preferably, in the step c, the spinning film is calcined for 2 hours at 250 ℃, which is favorable for stabilizing the multistage network structure of the prepared carbon fiber.
Preferably, in the step c, the temperature is raised to 800-1000 ℃ in a temperature programming mode, and the temperature raising rate is 3-5 ℃/min.
Further, in the step c, the temperature is raised to 900 ℃ in a temperature programming mode, and the temperature raising rate is 5 ℃/min.
The preferred carbonization temperature, heating rate and time are favorable for maintaining the multi-stage network structure of the spinning fiber and increasing the specific surface area of the carbon fiber.
The invention also provides a molybdenum sulfide/porous carbon nanofiber composite electrode material, which is prepared by the preparation method of the molybdenum sulfide/porous carbon nanofiber composite electrode material.
The invention also provides a perovskite solar cell which comprises the molybdenum sulfide/porous carbon nanofiber composite electrode material.
The molybdenum sulfide/porous carbon nanofiber composite electrode material provided by the invention has a multi-stage network porous structure, large specific surface area, strong conductivity and stable property, and the perovskite solar cell back electrode prepared by the material can enable a solar cell to have a more matched energy band structure, can serve as a hole transport layer while being used as a back electrode, improves carrier mobility, and is an ideal perovskite solar cell back electrode material, and the practical value is higher.
The invention also provides a preparation method of the perovskite solar cell, which comprises the following steps:
s101, uniformly mixing the molybdenum sulfide/porous carbon nanofiber composite electrode material with graphite, adding the mixture into terpineol, and ball-milling to obtain carbon slurry;
S102, uniformly mixing isopropyl titanate and absolute ethyl alcohol to obtain a dense-layer titanium dioxide solution; spin-coating the dense layer titanium dioxide solution on the surface of etched conductive glass, and annealing to obtain a perovskite dense layer;
s103, printing a porous titanium dioxide electron transport layer on the perovskite compact layer, and annealing to obtain a perovskite porous layer;
s104, dissolving lead iodide in N, N-dimethylformamide to obtain a lead iodide solution;
Dissolving iodomethylamine in isopropanol to obtain iodomethylamine solution;
spin-coating a lead iodide solution and an iodomethylamine solution on the perovskite porous layer in sequence from bottom to top, and annealing to obtain a perovskite absorption layer;
And S105, scraping the carbon paste on the surface of the perovskite absorption layer, and annealing to obtain the perovskite solar cell.
The preparation method of the perovskite solar cell back electrode provided by the invention is simple, low in cost, free of special equipment, suitable for large-scale production and application, and beneficial to realizing commercial application of the perovskite solar cell.
Preferably, in step S101, the mass ratio of the molybdenum sulfide/porous carbon nanofiber composite electrode material, graphite and terpineol is 3:1:10-15.
Preferably, in step S101, the rotation speed of the ball milling is 300rpm-500rpm, and the ball milling time is 12h-36h.
Illustratively, in step S101, an omnibearing planetary ball mill is used for ball milling.
In step S102, the etching of the conductive glass may be performed by a conventional etching method in the art, and the specific method for etching the conductive glass is: sticking adhesive tapes on two sides of the conductive glass, reserving an etching line with the width of 1mm in the middle, uniformly spreading zinc powder on the etching line, dipping 12mol/L concentrated hydrochloric acid with a cotton swab, and dripping the concentrated hydrochloric acid on the zinc powder to enable the concentrated hydrochloric acid to react with the zinc powder to etch the conductive film on the conductive glass substrate; and sequentially ultrasonically cleaning the etched conductive glass substrate by using a detergent water solution, deionized water, acetone, isopropanol and absolute ethyl alcohol for 10-30 min.
Optionally, in step S102, the conductive glass may be fluorine doped tin oxide transparent conductive glass, indium tin oxide transparent conductive glass, aluminum doped zinc oxide transparent conductive glass, transparent indium tin oxide conductive film, or transparent cadmium telluride conductive film.
Preferably, in step S102, the volume ratio of isopropyl titanate to absolute ethanol is 1:4-6.
Illustratively, in step S102, a spin coating machine is used to spin-coat a dense layer of titanium dioxide solution on the etched conductive glass surface, and the spin coating is performed for 20S-40S at 5000rpm-7000rpm, and the spin coating amount is 30 mu L-50 mu L.
Preferably, in step S102, the annealing temperature is 450-550 ℃ and the annealing time is 100-150 min.
Preferably, in step S103, the annealing temperature is 400-500 ℃ and the annealing time is 20-40 min.
Illustratively, in step S103, a porous titania electron transport layer is screen printed on the perovskite dense layer.
Optionally, in step S104, the concentration of the lead iodide solution is 0.6-0.8g/mL, and the concentration of the iodomethylamine solution is 48-52mg/mL.
Alternatively, in step S104, the spin-coating amount of the lead iodide solution is 30. Mu.L to 50. Mu.L, and the spin-coating amount of the iodomethylamine solution is 30. Mu.L to 50. Mu.L.
After spin-coating the lead iodide solution, the solution was left to stand for 15 to 25 seconds, and then the iodomethylamine solution was spin-coated.
Illustratively, in step S104, the spin-coated lead iodide solution and the iodomethylamine solution are spun at 2500rpm to 4000rpm, and the spin-coating time of each solution is 15S to 30S.
Preferably, in step S104, the annealing temperature is 140-160 ℃ and the annealing time is 15-25 min.
Illustratively, in step S105, the thickness of the blade-coated carbon paste is 50 μm to 70 μm, and the blade-coated area is 1 x 1cm 2.
Preferably, in step S105, the annealing temperature is 50-100 ℃ and the annealing time is 0.5-1 h.
The perovskite solar cell film layer provided by the invention has the advantages of simple preparation method, low cost, no need of special equipment, suitability for large-scale production and application, and suitability for realizing the commercialization application of perovskite solar cells.
Drawings
FIG. 1 is an SEM image of a molybdenum sulfide/porous carbon nanofiber composite electrode material prepared in example 1 of the present invention;
FIG. 2 is a J-V curve of a perovskite solar cell prepared as example 1 of the invention;
FIG. 3 is an SEM image of the carbon nanofiber material prepared in comparative example 1 of the present invention;
FIG. 4 is a J-V curve of the perovskite solar cell prepared according to comparative example 1 of the invention;
FIG. 5 is an SEM image of the silica/porous carbon nanofiber composite electrode material prepared in comparative example 2 of the present invention;
fig. 6 is a J-V curve of the perovskite solar cell prepared according to comparative example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In order to better illustrate the present invention, the following examples are provided for further illustration.
Example 1
The embodiment of the invention provides a preparation method of a molybdenum sulfide/porous carbon nanofiber composite electrode material, which comprises the following steps:
step a, weighing 0.5g of polyacrylonitrile and 0.1g of ammonium tetrathiomolybdate ((NH 4)2MoS4), adding into 5mL of N, N-dimethylformamide, and magnetically stirring at normal temperature until the mixture is clear and transparent to obtain spinning solution;
step b, transferring the spinning solution into an electrostatic spinning instrument for electrostatic spinning to obtain a spinning film; wherein the loading voltage is 18kV, the distance between the spray head and the aluminum foil is 15cm, the flow rate is 1.2mL/h, and the humidity is 30%;
And c, calcining the spinning film at 250 ℃ for 2 hours in an air atmosphere, transferring the spinning film into a tube furnace, heating to 900 ℃ at a speed of 5 ℃/min in an inert atmosphere, and carbonizing for 2 hours to obtain the molybdenum sulfide/porous carbon nanofiber composite electrode material.
The prepared molybdenum sulfide/porous carbon nanofiber composite electrode material is prepared into a perovskite solar cell, and the specific steps are as follows:
s101, weighing 0.3g of the prepared molybdenum sulfide/porous carbon nanofiber composite electrode material, uniformly mixing 0.1g of graphite, adding into 1.2g of terpineol, and ball-milling for 24 hours by adopting an omnibearing planetary ball mill at a rotating speed of 400rpm to obtain carbon slurry;
S102, sticking adhesive tapes on two sides of the conductive glass, reserving an etching line with the width of 1mm in the middle, uniformly spreading zinc powder on the etching line, dipping 12mol/L concentrated hydrochloric acid with a cotton swab, and dripping the concentrated hydrochloric acid on the zinc powder to enable the concentrated hydrochloric acid to react with the zinc powder to etch a conductive film on a conductive glass substrate; sequentially ultrasonically cleaning the etched conductive glass substrate for 20min by using a detergent water solution, deionized water, acetone, isopropanol and absolute ethyl alcohol to obtain etched conductive glass;
S103, measuring 8mL of isopropyl titanate and 40mL of absolute ethyl alcohol, and uniformly mixing to obtain a dense-layer titanium dioxide solution;
Placing the etched conductive glass on a sucker of a spin coater, dripping 40 mu L of dense layer titanium dioxide solution in the center of the conductive glass, spin-coating at 6000rpm for 30s, and annealing at 500 ℃ for 120min to obtain a perovskite dense layer;
s104, printing a porous titanium dioxide electron transport layer with the thickness of 700-1000nm on the perovskite compact layer by utilizing a screen printing method, and annealing for 30min at 450 ℃ in a muffle furnace to obtain a perovskite porous layer;
S105, dissolving 0.7g of lead iodide in 1mL of N, N-dimethylformamide to obtain a lead iodide solution;
50mg of iodomethylamine is dissolved in 1mL of isopropanol to obtain an iodomethylamine solution;
dropwise adding 40 mu L of lead iodide solution on the perovskite porous layer, spin-coating, waiting for 15-25s, dropwise adding 40 mu L of iodomethylamine solution, continuing spin-coating, and annealing at 150 ℃ for 20min at Wen Tai ℃ to obtain a perovskite absorption layer;
S106, the carbon paste is scraped on the surface of the perovskite absorption layer, the thickness of the carbon paste is 50-70 mu m, the scraping area is 1 x 1cm 2, and the perovskite solar cell is obtained after annealing for 1h at 80 ℃.
An SEM image of the molybdenum sulfide/porous carbon nanofiber composite electrode material prepared in this example is shown in fig. 1, and a J-V curve of the perovskite solar cell is shown in fig. 2.
Example 2
The embodiment of the invention provides a preparation method of a molybdenum sulfide/porous carbon nanofiber composite electrode material, which comprises the following steps:
Step a, weighing 0.4g of polyacrylonitrile and 0.1g of ammonium tetrathiomolybdate ((NH 4)2MoS4), adding into 4mL of N, N-dimethylformamide, and magnetically stirring at normal temperature until the mixture is clear and transparent to obtain spinning solution;
Step b, transferring the spinning solution into an electrostatic spinning instrument for electrostatic spinning to obtain a spinning film; wherein the loading voltage is 15kV, the distance between the spray head and the aluminum foil is 18cm, the flow rate is 1mL/h, and the humidity is 25%;
And c, calcining the spinning film at 200 ℃ for 3 hours in an air atmosphere, transferring the spinning film into a tube furnace, heating to 800 ℃ at a speed of 3 ℃/min in an inert atmosphere, and carbonizing for 3 hours to obtain the molybdenum sulfide/porous carbon nanofiber composite electrode material.
The prepared molybdenum sulfide/porous carbon nanofiber composite electrode material is prepared into a perovskite solar cell, and the specific steps are as follows:
s101, weighing 0.3g of the prepared molybdenum sulfide/porous carbon nanofiber composite electrode material, uniformly mixing 0.1g of graphite, adding into 1.0g of terpineol, and ball-milling for 36 hours at a rotating speed of 300rpm by adopting an omnibearing planetary ball mill to obtain carbon slurry;
S102, sticking adhesive tapes on two sides of the conductive glass, reserving an etching line with the width of 1mm in the middle, uniformly spreading zinc powder on the etching line, dipping 12mol/L concentrated hydrochloric acid with a cotton swab, and dripping the concentrated hydrochloric acid on the zinc powder to enable the concentrated hydrochloric acid to react with the zinc powder to etch a conductive film on a conductive glass substrate; sequentially ultrasonically cleaning the etched conductive glass substrate for 10min by using a detergent water solution, deionized water, acetone, isopropanol and absolute ethyl alcohol respectively to obtain etched conductive glass;
s103, measuring 8mL of isopropyl titanate and 32mL of absolute ethyl alcohol, and uniformly mixing to obtain a dense-layer titanium dioxide solution;
Placing the etched conductive glass on a sucker of a spin coater, dripping 30 mu L of dense layer titanium dioxide solution in the center of the conductive glass, spin-coating for 20s at 5000rpm, and annealing for 100min at 450 ℃ to obtain a perovskite dense layer;
s104, printing a porous titanium dioxide electron transport layer with the thickness of 700-1000nm on the perovskite compact layer by utilizing a screen printing method, and annealing for 20min at 500 ℃ in a muffle furnace to obtain a perovskite porous layer;
S105, dissolving 0.7g of lead iodide in 1mL of N, N-dimethylformamide to obtain a lead iodide solution;
50mg of iodomethylamine is dissolved in 1mL of isopropanol to obtain an iodomethylamine solution;
Dropwise adding 30 mu L of lead iodide solution on the perovskite porous layer, spin-coating, waiting for 15-25s, dropwise adding 30 mu L of iodomethylamine solution, continuing spin-coating, and annealing at 140 ℃ for 25min at Wen Tai ℃ to obtain a perovskite absorption layer;
s106, the carbon paste is scraped on the surface of the perovskite absorption layer, the thickness of the carbon paste is 50-70 mu m, the scraping area is 1 x 1cm 2, and the perovskite solar cell is obtained after annealing for 1h at 50 ℃.
Example 3
The embodiment of the invention provides a preparation method of a molybdenum sulfide/porous carbon nanofiber composite electrode material, which comprises the following steps:
Step a, weighing 0.6g of polyacrylonitrile and 0.1g of ammonium tetrathiomolybdate ((NH 4)2MoS4), adding into 5mL of N, N-dimethylformamide, and magnetically stirring at normal temperature until the mixture is clear and transparent to obtain spinning solution;
step b, transferring the spinning solution into an electrostatic spinning instrument for electrostatic spinning to obtain a spinning film; wherein the loading voltage is 20kV, the distance between the spray head and the aluminum foil is 20cm, the flow rate is 1.5mL/h, and the humidity is 35%;
And c, calcining the spinning film at 230 ℃ for 1h in an air atmosphere, transferring the spinning film into a tube furnace, heating to 1000 ℃ at a speed of 4 ℃/min in an inert atmosphere, and carbonizing for 1h to obtain the molybdenum sulfide/porous carbon nanofiber composite electrode material.
The prepared molybdenum sulfide/porous carbon nanofiber composite electrode material is prepared into a perovskite solar cell, and the specific steps are as follows:
S101, weighing 0.3g of the prepared molybdenum sulfide/porous carbon nanofiber composite electrode material, uniformly mixing 0.1g of graphite, adding into 1.5g of terpineol, and ball-milling for 12 hours at a rotating speed of 500rpm by adopting an omnibearing planetary ball mill to obtain carbon slurry;
S102, sticking adhesive tapes on two sides of the conductive glass, reserving an etching line with the width of 1mm in the middle, uniformly spreading zinc powder on the etching line, dipping 12mol/L concentrated hydrochloric acid with a cotton swab, and dripping the concentrated hydrochloric acid on the zinc powder to enable the concentrated hydrochloric acid to react with the zinc powder to etch a conductive film on a conductive glass substrate; sequentially ultrasonically cleaning the etched conductive glass substrate for 30min by using a detergent water solution, deionized water, acetone, isopropanol and absolute ethyl alcohol respectively to obtain etched conductive glass;
S103, measuring 8mL of isopropyl titanate and 48mL of absolute ethyl alcohol, and uniformly mixing to obtain a dense-layer titanium dioxide solution;
Placing the etched conductive glass on a sucker of a spin coater, dripping 50 mu L of dense layer titanium dioxide solution in the center of the conductive glass, spin-coating 40s at 7000rpm, and annealing at 550 ℃ for 100min to obtain a perovskite dense layer;
s104, printing a porous titanium dioxide electron transport layer with the thickness of 700-1000nm on the perovskite compact layer by utilizing a screen printing method, and annealing for 40min at 400 ℃ in a muffle furnace to obtain a perovskite porous layer;
S105, dissolving 0.7g of lead iodide in 1mL of N, N-dimethylformamide to obtain a lead iodide solution;
50mg of iodomethylamine is dissolved in 1mL of isopropanol to obtain an iodomethylamine solution;
Dropwise adding 50 mu L of lead iodide solution on the perovskite porous layer, spin-coating, waiting for 15-25s, dropwise adding 50 mu L of iodomethylamine solution, continuing spin-coating, and annealing at 160 ℃ Gao Wentai for 15min to obtain a perovskite absorption layer;
S106, the carbon paste is scraped on the surface of the perovskite absorption layer, the thickness of the carbon paste is 50-70 mu m, the scraping area is 1 x 1cm 2, and the perovskite solar cell is obtained after annealing for 0.5h at 100 ℃.
Comparative example 1
The comparative example provides a preparation method of a molybdenum sulfide/porous carbon nanofiber composite electrode material, which has the same steps as those of the example 1, except that ammonium tetrathiomolybdate is not added in the preparation process, and the specific steps are as follows:
weighing 0.5g of polyacrylonitrile and adding the polyacrylonitrile into 5ml of N, N-dimethylformamide, and magnetically stirring the mixture at normal temperature until the mixture is clear and transparent to obtain spinning solution;
step b, transferring the spinning solution into an electrostatic spinning instrument for electrostatic spinning to obtain a spinning film; wherein the loading voltage is 18kV, the distance between the spray head and the aluminum foil is 15cm, the flow rate is 1.2mL/h, and the humidity is 30%;
And c, calcining the spinning film at 250 ℃ for 2 hours in an air atmosphere, transferring the spinning film into a tube furnace, heating to 900 ℃ at a speed of 5 ℃/min in an inert atmosphere, and carbonizing for 2 hours to obtain the carbon nanofiber electrode material.
The carbon nanofiber material prepared above was fabricated into a perovskite solar cell in exactly the same manner as in example 1.
SEM images of the carbon nanofiber material prepared in this comparative example are shown in fig. 3, and J-V curves of the perovskite solar cell are shown in fig. 4.
Comparative example 2
The comparative example provides a method for preparing a silica/porous carbon nanofiber composite electrode material, which has the same steps as those of the example 1, except that ammonium tetrathiomolybdate in the step a is replaced by equal amount of silica, and the specific steps are as follows:
step a, weighing 0.5g of polyacrylonitrile and 0.25g of silicon dioxide, adding into 5mL of N, N-dimethylformamide, and magnetically stirring at normal temperature until the mixture is clear and transparent to obtain spinning solution;
step b, transferring the spinning solution into an electrostatic spinning instrument for electrostatic spinning to obtain a spinning film; wherein the loading voltage is 18kV, the distance between the spray head and the aluminum foil is 15cm, the flow rate is 1.2mL/h, and the humidity is 30%;
And c, calcining the spinning film at 250 ℃ for 2 hours in an air atmosphere, transferring the spinning film into a tube furnace, heating to 900 ℃ at a speed of 5 ℃/min in an inert atmosphere, and carbonizing for 2 hours to obtain the silicon dioxide/porous carbon nanofiber composite electrode material.
The prepared silica/porous carbon nanofiber composite electrode material was fabricated into a perovskite solar cell in exactly the same manner as in example 1.
SEM images of the silica/porous carbon nanofiber composite electrode materials prepared in this comparative example are shown in fig. 5, and J-V curves of perovskite solar cells are shown in fig. 6.
In order to better illustrate the characteristics of the molybdenum sulfide/porous carbon nanofiber composite electrode material provided by the embodiment of the invention, the perovskite solar cells prepared in the examples 1-3 and the comparative examples 1-2 are subjected to performance detection.
The perovskite solar cell prepared above was placed under a solar simulator (Abet Sun 3000) and subjected to photoelectric conversion efficiency test under standard light irradiation of 100mW/cm 2, the bias voltage was measured to be 1.25V-0.1V, and the effective area of the cell was 0.06cm 2. The test results are shown in Table 1.
TABLE 1
In summary, the perovskite solar cell prepared by the embodiment of the invention effectively improves the photoelectric conversion efficiency, and the perovskite solar cell prepared based on the method has the advantages of high efficiency, stability and low cost, and the development of the preparation technology provides a new device preparation strategy for the commercial application of the large-area perovskite solar cell.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (7)
1. The application of the molybdenum sulfide/porous carbon nanofiber composite electrode material as the back electrode of the large-area perovskite solar cell is characterized in that the preparation method of the molybdenum sulfide/porous carbon nanofiber composite electrode material comprises the following steps:
Step a, adding polyacrylonitrile and soluble molybdenum salt into N, N-dimethylformamide, and uniformly mixing to obtain spinning solution;
Step b, carrying out electrostatic spinning on the spinning solution to obtain a spinning film;
Step c, calcining the spinning film at 200-250 ℃ for 1-3 h, and carbonizing the spinning film at 800-1000 ℃ for 1-3 h in inert atmosphere to obtain the molybdenum sulfide/porous carbon nanofiber composite electrode material;
in the step a, the mass ratio of the polyacrylonitrile to the soluble molybdate is 4-6:1;
in the step a, the mass concentration of the polyacrylonitrile in the spinning solution is 8% -15%;
In step a, the soluble molybdenum salt is ammonium tetrathiomolybdate.
2. The use of the molybdenum sulfide/porous carbon nanofiber composite electrode material as a back electrode of a large area perovskite solar cell according to claim 1, wherein in step b, the parameters of the electrospinning are: the loading voltage is 15kV-20kV, the distance between the spray head and the aluminum foil is 15cm-20cm, the flow rate is 1mL/h-1.5mL/h, and the humidity is 25% -35%; and/or
In the step c, the temperature is raised to 800-1000 ℃ in a temperature programming mode, and the temperature raising rate is 3-5 ℃/min.
3. The molybdenum sulfide/porous carbon nanofiber composite electrode material is characterized by being prepared by the preparation method of the molybdenum sulfide/porous carbon nanofiber composite electrode material according to claim 1 or 2.
4. A perovskite solar cell, characterized by: a molybdenum sulfide/porous carbon nanofiber composite electrode material comprising the molybdenum sulfide/porous carbon nanofiber composite of claim 3.
5. The method for manufacturing a perovskite solar cell as claimed in claim 4, comprising the steps of:
s101, uniformly mixing the molybdenum sulfide/porous carbon nanofiber composite electrode material with graphite, adding the mixture into terpineol, and ball-milling to obtain carbon slurry;
S102, uniformly mixing isopropyl titanate and absolute ethyl alcohol to obtain a dense-layer titanium dioxide solution; spin-coating the dense layer titanium dioxide solution on the surface of etched conductive glass, and annealing to obtain a perovskite dense layer;
s103, printing a porous titanium dioxide electron transport layer on the perovskite compact layer, and annealing to obtain a perovskite porous layer;
s104, dissolving lead iodide in N, N-dimethylformamide to obtain a lead iodide solution;
Dissolving iodomethylamine in isopropanol to obtain iodomethylamine solution;
spin-coating a lead iodide solution and an iodomethylamine solution on the perovskite porous layer in sequence from bottom to top, and annealing to obtain a perovskite absorption layer;
And S105, scraping the carbon paste on the surface of the perovskite absorption layer, and annealing to obtain the perovskite solar cell.
6. The method for manufacturing a perovskite solar cell according to claim 5, wherein in the step S101, the mass ratio of the molybdenum sulfide/porous carbon nanofiber composite electrode material, graphite and terpineol is 3:1:10-15; and/or
In the step S101, the rotation speed of the ball milling is 300rpm-500rpm, and the ball milling time is 12h-36h; and/or
In the step S102, the volume ratio of the isopropyl titanate to the absolute ethyl alcohol is 1:4-6; and/or
In the step S102, the annealing temperature is 450-550 ℃ and the annealing time is 100-150 min.
7. The method of manufacturing a perovskite solar cell according to claim 5, wherein in step S103, the annealing temperature is 400 ℃ to 500 ℃ and the annealing time is 20min to 40min; and/or
In the step S104, the annealing temperature is 140-160 ℃ and the annealing time is 15-25 min;
in step S105, the annealing temperature is 50-100 ℃ and the annealing time is 0.5-1 h.
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