CN112768611A - Preparation method of trans-organic-inorganic hybrid perovskite solar cell - Google Patents
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Abstract
The invention discloses a preparation method of a trans-form organic-inorganic hybrid perovskite solar cell, which comprises an ITO conductive glass layer, a hole transport layer, a perovskite light absorption layer, an electron transport layer and an electrode layer from bottom to top in sequence. The preparation method comprises the steps of cleaning ITO conductive glass; preparing PEDOT with the thickness of 10-13 nm: agarose membrane, PEDOT: PSS solution spin coated on PEDOT: NiO is put on an agarose filmxThe aqueous dispersion of (a) was spin coated on PEDOT: obtaining 36-39 nm NiO on the PSS filmxFilm, get the hole transport layer; preparing a perovskite layer; dissolving PCEM in chlorobenzene, then spin-coating on the perovskite layer to obtain an electron transmission layer; and finally, evaporating a metal electrode with the thickness of 105-120 nm. The perovskite solar cell has higher photoelectric conversion efficiency and excellent stabilityAnd (4) sex.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a preparation method of a trans-form organic-inorganic hybrid perovskite solar cell.
Background
With the continuous development and progress of society, the demand of human beings for energy is also increasing. Solar energy is renewable, clean and environmentally friendly, compared to the non-renewable and environmentally polluting nature of traditional fossil energy sources. The traditional solar cell is represented by an amorphous silicon solar cell, but the amorphous silicon solar cell has high manufacturing cost, complicated manufacturing procedure and great pollution to the environment. The perovskite solar cell is a thin-film solar cell taking an organic-inorganic hybrid perovskite material as a light absorption layer. The organic-inorganic hybrid perovskite material has the outstanding advantages of high photoelectric conversion efficiency, low cost, simple manufacture and the like, and becomes one of the most promising solar cells.
The organic-inorganic hybrid perovskite solar cell with the traditional positive structure mainly comprises a photoanode (such as TiO)2+ABX3[A=CH3NH3(MA),B=Pb,X=I,Br,Cl]Perovskite light absorption material }, a hole transport layer (HTM) and a counter electrode, the photoelectric conversion efficiency of the perovskite solar cell is close to that of an amorphous silicon solar cell, but the hysteresis effect is obvious, and the stability of the device is to be improved. The trans-perovskite solar cell is formed by a hole transport layer/perovskite light absorption layer [ MAPbX [ ]3(X=I,Br,Cl)]Compared with an upright structure, the trans-structure has negligible hysteresis effect, and meanwhile, the flexible device can be prepared at low temperature, has good interface stability and is generally higher than an upright structure perovskite solar cell.
Poly (3, 4-ethylenedioxythiophene): poly (styrene sulfonate) (PEDOT: PSS) was first applied as a hole transport material in trans-perovskite devices, but PEDOT: the PSS solution is acidic and has a certain corrosion effect on an ITO electrode, wherein the PSS is mainly acidic and has strong water absorption, and most of perovskite materials are unstable in a humid environment, so that the stability and the efficiency of perovskite are influenced to a certain extent.
Disclosure of Invention
Based on the fact that in the trans-perovskite solar cell in the prior art, poly (styrene sulfonate) (PSS) in a hole transport layer has acidity, can corrode an ITO electrode and has strong water absorption, and affects the photoelectric conversion efficiency of the solar cell, the invention aims to provide a preparation method of a trans-organic-inorganic hybrid perovskite solar cell, which comprises the following steps:
s1: and (2) adding deionized water into ITO conductive glass, adding Alconox lotion powder, heating to 80-90 ℃, dissolving the lotion completely, performing ultrasonic washing for 30-50 min, performing ultrasonic washing for 10-16 times by using deionized water, performing ultrasonic washing for 25-30 min by using acetone and ethanol respectively in sequence, and drying for 30min at 80-90 ℃ for later use.
S2: adding PEDOT (poly (3, 4-ethylenedioxythiophene)): agarose was added to dimethylsulfoxide and N, N-dimethylformamide, and then an ITO substrate was placed on a spin coater, PEDOT: and spin-coating an agarose solution on an ITO substrate, and then placing the ITO substrate at 100-120 ℃ for annealing for 10-15 min to form PEDOT with the thickness of 10-13 nm: agarose membranes.
S2-1: and (3) mixing PEDOT: the PSS solution was spin coated on PEDOT at step S2: annealing the agarose film for 8-12 min at 120-150 ℃ to form a 6-9 nm PEDOT layer: PSS film.
S2-2: NiO is mixedxSpin coating the aqueous dispersion of (3) on the substrate at step S2-1 PEDOT: coating the PSS film at the spin coating speed of 4000rpm/s for 12-15 s, repeating the spin coating for 3 times, and finally annealing at 125-140 ℃ for 15min to obtain 36-39 nm NiOxA film.
S3: will CH3NH3I、PbI2Adding into dimethyl sulfoxide and N, N-dimethylformamide, and ultrasonic dissolving to obtain CH3NH3I、PbI2Dimethyl sulfoxide and N, N-dimethylformamide in a molar ratio of 1:1:1: 1.2-3.6, and spin-coating NiO obtained in the step S2-2xAnd (3) on the film, wherein the spin-coating speed is 4000-7000 rpm/s, the spin-coating time is 10-30 s, the spin-coating is repeated for 4-6 times, a toluene solvent is dropwise added after each spin-coating is finished, and finally annealing is carried out at 100-110 ℃ for 10-15 min to obtain the perovskite layer.
S4: and (3) dissolving PCEM in chlorobenzene, spin-coating on the perovskite layer obtained in the step S3 at the spin-coating speed of 1500-2000 rpm/S for 30-50S, and annealing at 70-80 ℃ for 8-12 min to obtain the electron transmission layer.
S5: step S4, a metal electrode layer is deposited, wherein the thickness of the metal electrode layer is 105-120 nm.
Preferably, the proportion of the PEDOT (poly (3, 4-ethylenedioxythiophene)) to the agarose is 40-65%: 33 to 62 percent.
Preferably, the volume ratio of the dimethyl sulfoxide to the N, N-dimethylformamide is (1-2) to (3.5-5).
Preferably, NiO is used as the abovexThe preparation method comprises the following steps:
adding nickel chloride hexahydrate into deionized water, performing ultrasonic treatment, dropwise adding a sodium hydroxide solution, adjusting the pH value of the solution, performing ultrasonic treatment for 20-30 min, standing for 15min, centrifuging, separating, washing with deionized water, performing vacuum drying on the solid at 80-90 ℃, then placing the solid in a tube furnace, and performing annealing treatment at 275-292 ℃ for 2.5-4 h to obtain NiOx。
More preferably, the pH value is adjusted to be within the range of 10 to 10.6.
Preferably, the metal electrode layer is a metal silver electrode layer or a metal gold electrode layer.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a hole transport layer of the trans-perovskite solar cell adopts PEDOT: agarose film/PEDOT: PSS film/NiOxThe perovskite solar cell is prepared in a thin film combination mode, and the thickness of the three-layer film is controlled in the preparation process, so that the prepared perovskite solar cell has the optimal photoelectric conversion efficiency; by combining the three films, the conversion efficiency and the stability of the film can be effectively improved.
Drawings
Fig. 1 is an SEM image of a hole transport layer of a perovskite solar cell prepared in example 1 of the present invention.
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of a trans-form organic-inorganic hybrid perovskite solar cell specifically comprises the following steps:
s1: and adding ITO conductive glass deionized water into Alconox lotion powder, heating to 80 ℃, dissolving the lotion completely, performing ultrasonic treatment for 30min, then performing ultrasonic treatment for 10 times by using the deionized water, finally performing ultrasonic treatment for 25min by using acetone and ethanol respectively in sequence, and drying for 30min at 80 ℃ for later use.
S2: adding PEDOT (poly (3, 4-ethylenedioxythiophene)): agarose was added to dimethylsulfoxide and N, N-dimethylformamide, and then an ITO substrate was placed on a spin coater, PEDOT: the agarose solution was spin coated on an ITO substrate and then left to anneal at 100 ℃ for 10min to form a 10nm thick PEDOT: agarose membrane, in which PEDOT (poly (3, 4-ethylenedioxythiophene)) and agarose were added in a ratio of 40%: 60 percent; the volume ratio of the dimethyl sulfoxide to the N, N-dimethylformamide is 1: 3.5.
S2-1: and (3) mixing PEDOT: the PSS solution was spin coated on PEDOT at step S2: annealing on agarose membrane at 120 ℃ for 8min to form a layer of 6nm PEDOT: PSS film.
S2-2: NiO is mixedxSpin coating the aqueous dispersion of (3) on the substrate at step S2-1 PEDOT: coating the PSS film with spin coating speed of 4000rpm/s for 12s, repeating the spin coating for 3 times, and annealing at 125 deg.C for 15min to obtain 36nm NiOxA film.
S3: will CH3NH3I、PbI2Adding into dimethyl sulfoxide and N, N-dimethylformamide, and ultrasonic dissolving to obtain CH3NH3I、PbI2Dimethyl sulfoxide and N, N-dimethylformamide in a molar ratio of 1:1:1:1.2, and then spin-coating the NiO in step S2-2xAnd (3) repeatedly spin-coating the film for 4 times at the spin-coating speed of 4000rpm/s and the spin-coating time of 10s, dropwise adding a toluene solvent after each spin-coating, and finally annealing at 100 ℃ for 10min to obtain the perovskite layer.
S4: the PCEM was dissolved in chlorobenzene, and then spin-coated on the perovskite layer of step S3 at a spin-coating speed of 1500rpm/S for 30S, followed by annealing at 70 ℃ for 8min to obtain an electron transport layer.
S5: and step S4, evaporating a metal silver electrode layer, wherein the thickness of the metal electrode layer is 105 nm.
Example 2
A preparation method of a trans-form organic-inorganic hybrid perovskite solar cell specifically comprises the following steps:
s1: and adding ITO conductive glass deionized water into Alconox lotion powder, heating to 90 ℃, dissolving the lotion completely, performing ultrasonic treatment for 50min, then performing ultrasonic washing for 16 times by using the deionized water, finally performing ultrasonic washing for 30min by using acetone and ethanol respectively in sequence, and drying for 30min at 90 ℃ for later use.
S2: adding PEDOT (poly (3, 4-ethylenedioxythiophene)): agarose was added to dimethylsulfoxide and N, N-dimethylformamide, and then an ITO substrate was placed on a spin coater, PEDOT: the agarose solution was spin coated on an ITO substrate and then left to anneal at 120 ℃ for 15min to form 13nm thick PEDOT: agarose membrane, in which PEDOT (poly (3, 4-ethylenedioxythiophene)) and agarose were added at a ratio of 45%: 55 percent; the volume ratio of the dimethyl sulfoxide to the N, N-dimethylformamide is 2: 5.
S2-1: and (3) mixing PEDOT: the PSS solution was spin coated on PEDOT at step S2: annealing on agarose membrane at 150 ℃ for 12min to form a layer of 9nm PEDOT: PSS film.
S2-2: NiO is mixedxSpin coating the aqueous dispersion of (3) on the substrate at step S2-1 PEDOT: coating the PSS film at 4000rpm/s for 15s, repeating the coating for 3 times, and annealing at 140 deg.C for 15min to obtain 39nm NiOxA film.
S3: will CH3NH3I、PbI2Adding into dimethyl sulfoxide and N, N-dimethylformamide, and ultrasonic dissolving to obtain CH3NH3I、PbI2Dimethyl sulfoxide and N, N-dimethylformamide in a molar ratio of 1:1:1:3.6, and then spin-coating the NiO in step S2-2xAnd (3) repeatedly spin-coating the film for 6 times at the spin-coating speed of 7000rpm/s and the spin-coating time of 30s, dropwise adding a toluene solvent after each spin-coating, and finally annealing at 110 ℃ for 15min to obtain the perovskite layer.
S4: the PCEM was dissolved in chlorobenzene, then spin-coated on the perovskite layer of step S3 at a spin-coating speed of 2000rpm/S for 50S, and then annealed at 80 ℃ for 12min to obtain an electron transport layer.
S5: and step S4, evaporating a metal gold electrode layer, wherein the thickness of the metal electrode layer is 120 nm.
Example 3
A preparation method of a trans-form organic-inorganic hybrid perovskite solar cell specifically comprises the following steps:
s1: and adding ITO conductive glass deionized water into Alconox lotion powder, heating to 85 ℃, dissolving the lotion completely, performing ultrasonic treatment for 40min, then performing ultrasonic treatment for 12 times by using the deionized water, finally performing ultrasonic treatment for 25min by using acetone and ethanol respectively in sequence, and drying for 30min at 85 ℃ for later use.
S2: adding PEDOT (poly (3, 4-ethylenedioxythiophene)): agarose was added to dimethylsulfoxide and N, N-dimethylformamide, and then an ITO substrate was placed on a spin coater, PEDOT: the agarose solution was spin coated on an ITO substrate and then left to anneal at 110 ℃ for 12min to form an 11nm thick PEDOT: agarose membrane, in which PEDOT (poly (3, 4-ethylenedioxythiophene)) and agarose were added in a proportion of 48%: 52 percent; the volume ratio of the dimethyl sulfoxide to the N, N-dimethylformamide is 1.4: 4.2.
S2-1: and (3) mixing PEDOT: the PSS solution was spin coated on PEDOT at step S2: annealing on agarose membrane at 125 deg.C for 10min to form a layer of 7nm PEDOT: PSS film.
S2-2: NiO is mixedxSpin coating the aqueous dispersion of (3) on the substrate at step S2-1 PEDOT: coating the PSS film at 4000rpm/s for 13s, repeating the coating for 3 times, and annealing at 130 deg.C for 15min to obtain 37nm NiOxA film.
S3: will CH3NH3I、PbI2Adding into dimethyl sulfoxide and N, N-dimethylformamide, and ultrasonic dissolving to obtain CH3NH3I、PbI2Dimethyl sulfoxide and N, N-dimethylformamide in a molar ratio of 1:1:1:2.5, and then spin-coating the NiO in step S2-2xSpin coating on a thin film, wherein the spin coating speed is 5000rpm/sThe time is 20s, the spin coating is repeated for 5 times, the toluene solvent is dripped after each spin coating is finished, and finally the annealing is carried out for 12min at the temperature of 105 ℃, so as to obtain the perovskite layer.
S4: the PCEM was dissolved in chlorobenzene, then spin-coated on the perovskite layer of step S3 at a spin-coating speed of 1700rpm/S for 40S, and then annealed at 75 ℃ for 10min to obtain an electron transport layer.
S5: and step S4, evaporating a metal silver electrode layer, wherein the thickness of the metal electrode layer is 110 nm.
Example 4
A preparation method of a trans-form organic-inorganic hybrid perovskite solar cell specifically comprises the following steps:
s1: and adding ITO conductive glass deionized water into Alconox lotion powder, heating to 88 ℃, dissolving the lotion completely, performing ultrasonic treatment for 45min, then performing ultrasonic washing for 14 times by using the deionized water, finally performing ultrasonic washing for 30min by using acetone and ethanol respectively in sequence, and drying for 30min at 90 ℃ for later use.
S2: adding PEDOT (poly (3, 4-ethylenedioxythiophene)): agarose was added to dimethylsulfoxide and N, N-dimethylformamide, and then an ITO substrate was placed on a spin coater, PEDOT: the agarose solution was spin coated on an ITO substrate and then left to anneal at 115 ℃ for 14min to form a 12nm thick PEDOT: agarose membrane, in which PEDOT (poly (3, 4-ethylenedioxythiophene)) and agarose were added in a ratio of 55%: 45 percent; the volume ratio of the dimethyl sulfoxide to the N, N-dimethylformamide is 1.8: 4.6.
S2-1: and (3) mixing PEDOT: the PSS solution was spin coated on PEDOT at step S2: annealing on agarose membrane at 130 ℃ for 11min to form a layer of 8nm PEDOT: PSS film.
S2-2: NiO is mixedxSpin coating the aqueous dispersion of (3) on the substrate at step S2-1 PEDOT: coating the PSS film with spin coating speed of 4000rpm/s for 14s, repeating the spin coating for 3 times, and annealing at 135 deg.C for 15min to obtain 38nm NiOxA film.
S3: will CH3NH3I、PbI2Adding into dimethyl sulfoxide and N, N-dimethylformamide, and ultrasonic dissolving to obtain CH3NH3I、PbI2Dimethyl sulfoxide and N, N-dimethylformamide in a molar ratio of 1:1:1:3.4, and then spin-coating the NiO in step S2-2xAnd (3) repeatedly spin-coating the film for 6 times at the spin-coating speed of 6000rpm/s and the spin-coating time of 25s, dropwise adding a toluene solvent after each spin-coating, and finally annealing at 110 ℃ for 14min to obtain the perovskite layer.
S4: the PCEM was dissolved in chlorobenzene, then spin-coated on the perovskite layer of step S3 at a spin-coating speed of 1800rpm/S for 45S, and then annealed at 80 ℃ for 11min to obtain an electron transport layer.
S5: and step S4, evaporating a metal gold electrode layer, wherein the thickness of the metal electrode layer is 115 nm.
Comparative example 1
A preparation method of a trans-perovskite solar cell specifically comprises the following steps:
s1: and adding ITO conductive glass deionized water into Alconox lotion powder, heating to 80 ℃, dissolving the lotion completely, performing ultrasonic treatment for 30min, then performing ultrasonic treatment for 10 times by using the deionized water, finally performing ultrasonic treatment for 25min by using acetone and ethanol respectively in sequence, and drying for 30min at 80 ℃ for later use.
S2: and (3) mixing PEDOT: the PSS solution was spin coated on PEDOT at step S2: annealing on agarose membrane at 120 ℃ for 8min to form a layer of 6nm PEDOT: PSS film.
S3: will CH3NH3I、PbI2Adding into dimethyl sulfoxide and N, N-dimethylformamide, and ultrasonic dissolving to obtain CH3NH3I、PbI2Dimethyl sulfoxide and N, N-dimethylformamide in a molar ratio of 1:1:1:1.2, and then spin-coating the NiO in step S2-2xAnd (3) repeatedly spin-coating the film for 4 times at the spin-coating speed of 4000rpm/s and the spin-coating time of 10s, dropwise adding a toluene solvent after each spin-coating, and finally annealing at 100 ℃ for 10min to obtain the perovskite layer.
S4: the PCEM was dissolved in chlorobenzene, and then spin-coated on the perovskite layer of step S3 at a spin-coating speed of 1500rpm/S for 30S, followed by annealing at 70 ℃ for 8min to obtain an electron transport layer.
S5: and step S4, evaporating a metal silver electrode layer, wherein the thickness of the metal electrode layer is 105 nm.
Experimental example:
the perovskite solar cells prepared in examples 1 to 4 and comparative example 1 were subjected to performance tests, and the test results are shown in table 1,
table 1. test results:
as can be seen from table 1 above, the open-circuit voltages of the trans-form inorganic-organic perovskite solar cells prepared in embodiments 1 to 4 of the present invention are all above 1.09V, and compared with the perovskite solar cell in comparative example 1, the trans-form inorganic-organic perovskite solar cell has a higher open-circuit voltage and a higher photoelectric conversion efficiency.
The perovskite solar cells prepared in examples 1 to 4 and comparative example 1 were subjected to the performance test of photoelectric conversion efficiency again after 60 days, and the test results are shown in table 2,
table 2.test photoelectric conversion efficiency results after 60 days:
as can be seen from table 2, the photoelectric conversion efficiency of the perovskite solar cells prepared in embodiments 1 to 4 of the invention is over 17.2%, and compared with the perovskite solar cell in comparative example 1, the perovskite solar cell has better stability.
Claims (6)
1. A preparation method of a trans-form organic-inorganic hybrid perovskite solar cell comprises an ITO conductive glass layer, a hole transport layer, a perovskite light absorption layer, an electron transport layer and an electrode layer from bottom to top in sequence, and is characterized by comprising the following steps:
s1: deionized water is added into ITO conductive glass, Alconox lotion powder is added, the mixture is heated to 80-90 ℃, the lotion is completely dissolved, ultrasonic washing is carried out for 30-50 min, then deionized water is used for ultrasonic washing for 10-16 times, finally acetone and ethanol are used for ultrasonic washing respectively for 25-30 min in sequence, and drying is carried out for 30min at 80-90 ℃ for later use;
s2: adding PEDOT (poly (3, 4-ethylenedioxythiophene)): agarose was added to dimethylsulfoxide and N, N-dimethylformamide, and then an ITO substrate was placed on a spin coater, PEDOT: and spin-coating an agarose solution on an ITO substrate, and then placing the ITO substrate at 100-120 ℃ for annealing for 10-15 min to form PEDOT with the thickness of 10-13 nm: an agarose membrane;
s2-1: and (3) mixing PEDOT: the PSS solution was spin coated on PEDOT at step S2: annealing the agarose film for 8-12 min at 120-150 ℃ to form a 6-9 nm PEDOT layer: a PSS film;
s2-2: NiO is mixedxSpin coating the aqueous dispersion of (3) on the substrate at step S2-1 PEDOT: coating the PSS film at the spin coating speed of 4000rpm/s for 12-15 s, repeating the spin coating for 3 times, and finally annealing at 125-140 ℃ for 15min to obtain 36-39 nm NiOxA film;
s3: will CH3NH3I、PbI2Adding into dimethyl sulfoxide and N, N-dimethylformamide, and ultrasonic dissolving to obtain CH3NH3I、PbI2Dimethyl sulfoxide and N, N-dimethylformamide in a molar ratio of 1:1:1: 1.2-3.6, and spin-coating NiO obtained in the step S2-2xOn a film, repeatedly spin-coating for 4-6 times at a spin-coating speed of 4000-7000 rpm/s and a spin-coating time of 10-30 s, dropwise adding a toluene solvent after each spin-coating, and finally annealing at 100-110 ℃ for 10-15 min to obtain a perovskite layer;
s4: dissolving PCEM in chlorobenzene, spin-coating on the perovskite layer obtained in the step S3 at the spin-coating speed of 1500-2000 rpm/S for 30-50S, and annealing at 70-80 ℃ for 8-12 min to obtain an electron transmission layer;
s5: step S4, a metal electrode layer is deposited, wherein the thickness of the metal electrode layer is 105-120 nm.
2. The method for preparing a trans-organic-inorganic hybrid perovskite solar cell as claimed in claim 1, wherein the addition ratio of PEDOT (poly (3, 4-ethylenedioxythiophene)) to agarose is 40-65%: 33 to 62 percent.
3. The method for preparing a trans-organic-inorganic hybrid perovskite solar cell as claimed in claim 1, wherein the volume ratio of dimethyl sulfoxide to N, N-dimethylformamide is (1-2) to (3.5-5).
4. The method for preparing a trans-organic-inorganic hybrid perovskite solar cell as claimed in claim 1, wherein the NiO isxThe preparation method comprises the following steps:
adding nickel chloride hexahydrate into deionized water, performing ultrasonic treatment, dropwise adding a sodium hydroxide solution, adjusting the pH value of the solution, performing ultrasonic treatment for 20-30 min, standing for 15min, centrifuging, separating, washing with deionized water, performing vacuum drying on the solid at 80-90 ℃, then placing the solid in a tube furnace, and performing annealing treatment at 275-292 ℃ for 2.5-4 h to obtain NiOx。
5. The method for preparing a trans-organic-inorganic hybrid perovskite solar cell according to claim 4, wherein the pH value is adjusted to be within a range of 10-10.6.
6. The method for preparing a trans-organic-inorganic hybrid perovskite solar cell according to claim 1, wherein the metal electrode layer is a metal silver electrode layer or a metal gold electrode layer.
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