CN114203906A - Preparation method and application of perovskite film - Google Patents

Preparation method and application of perovskite film Download PDF

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CN114203906A
CN114203906A CN202111517985.1A CN202111517985A CN114203906A CN 114203906 A CN114203906 A CN 114203906A CN 202111517985 A CN202111517985 A CN 202111517985A CN 114203906 A CN114203906 A CN 114203906A
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lead
bismuth
inorganic halogen
iodide
halogen salt
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王康
马思敏
薛小洋
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North Minzu University
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    • H—ELECTRICITY
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    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
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    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
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Abstract

A preparation method and application of a perovskite film are used for solving the technical problem that how to have better photoelectric conversion efficiency and better stability of the existing perovskite film. Preparing an intermediate material containing bismuth by using inorganic halogen salt containing bismuth, N-dimethylformamide solution, hydroiodic acid and raw materials, preparing a precursor solution by using the intermediate material as a raw material and using the inorganic halogen salt containing lead, cesium iodide and N, N-dimethylformamide solution as raw materials, and preparing a perovskite film by using the precursor solution, wherein the perovskite crystal has the structure of ABX3The perovskite film has good stability, the photoelectric conversion rate can exceed 10%, and the black perovskite film can be obtained at the temperature of 80-150 ℃; the invention is mainly used in the technical field of photoelectric functional materials and devices.

Description

Preparation method and application of perovskite film
Technical Field
The invention relates to the technical field of photoelectric functional materials and devices, in particular to a preparation method and application of a perovskite film.
Background
With the continuous development of science and technology, environmental pollution and energy crisis are increasingly aggravated, solar batteries using solar energy have outstanding advantages of cleanness, high efficiency, sustainability and the like, and are paid much attention as leaders of third-generation solar batteries
The development of organic/inorganic hybrid perovskite solar cells is the most rapid; perovskite is used as an optoelectronic material, has large spectral absorption intensity and wide spectral absorption range, and can efficiently absorb most of energy in solar energy.
Existing alpha-Cs prepared from lead-containing inorganic halogen saltsxDMF1-XPbIz1Brz2Cl3-z1-z2The photoelectric conversion efficiency of the solar cell made of the film is more than 16 percent, the lead-containing inorganic halogen salt mainly comprises lead iodide, lead bromide and lead chloride, the absorption intensity and the absorption range of the material to sunlight can be well adjusted by adjusting the proportion of three elements of Cl, Br and I in the lead-containing inorganic halogen salt in the perovskite material, and the prior art discloses that the alpha-Cs prepared by binary blending of Cl, Br and I is adjustedxDMF1-XPbIz1Brz2Cl3-z1-z2The film also has higher photoelectric conversion efficiency, but has poor stability, and can be easily phase-changed into Cs without photovoltaic activity at room temperaturexDMF1-XPbIz1Brz2Cl3-z1-z2Thin film, and the black perovskite film can be generated only under the condition of more than 200 ℃.
With respect to ternary blended systems of perovskite photovoltaic cells, patent publication No. CN104332560B discloses synthesis of iodomethylamine and bromomethylamine with PbCl2，PbBr2，PbI2Adjusting the molar ratio, dissolving in N-N dimethylformamide, and using as light absorption layer material to prepare photovoltaic cell, wherein MAPbBr isyI1-x-yClxCell relative to MAPbI1-xClxThe open-circuit voltage of the battery is improved to a certain extent by introducing Br, but the short-circuit current and the conversion efficiency are greatly reduced, and the maximum efficiency of the ternary blended thin film battery is 3.9 percent.
Disclosure of Invention
The invention aims to provide a preparation method and application of a perovskite film aiming at the defects of the prior art, and aims to solve the technical problem of how to have better photoelectric conversion efficiency and better stability of the conventional perovskite film.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a perovskite film comprises the following steps:
(1) dissolving inorganic halogen salt containing bismuth in N, N-dimethylformamide solution;
(2) dropwise adding hydroiodic acid after the bismuth-containing inorganic halogen salt in the step (1) is dissolved, and stirring to obtain a light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2), transferring the light yellow precipitate into a container, and washing the light yellow precipitate with anhydrous ether;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
(5) weighing the intermediate material in the step (4), weighing lead-containing inorganic halogen salt and cesium iodide, and dissolving all the raw materials into an N, N-dimethylformamide solution to obtain a precursor solution;
(6) depositing the precursor solution in the step (5) on a substrate;
(7) carrying out thermal annealing treatment on the substrate in the step (6) to form a black perovskite film;
wherein the inorganic halogen salt containing bismuth is one or a mixture of more than one of bismuth iodide, bismuth chloride and bismuth bromide;
the lead-containing inorganic halogen salt is lead iodide or a mixture of more than one of lead iodide, lead chloride and lead bromide, and one of the mixtures is lead iodide;
the intermediate material has the general formula: DMABiIz1Brz2Cl3-z1-z2；
The general formula of the precursor solution is as follows: csxDMA1-xBiyPb1-yIz1Brz2Cl3-z1-z2，(x≠0、x≠1；y≠0、y≠1；z1≠0,z2≠0)。
Further, the inorganic halogen salt containing bismuth is bismuth bromide, and the inorganic halogen salt containing lead is lead iodide.
Further, the thermal annealing treatment temperature in the step (7) is 80-150 ℃, and the annealing time is 5 min.
Further, the mass ratio of the precursor material, the lead-containing inorganic halogen salt and the cesium iodide in the step (5) is (1.5-2.5): (2-2.5): (0.5 to 1).
Further, the mass of the lead iodide in the lead-containing inorganic halogen salt mixture in the step (1) is 80-90% of the total mass of the mixture.
Further, in the step (6), a spin coater is adopted to deposit the precursor solution on the substrate, wherein the spin coater has a rotation speed of 4000 revolutions per second and a rotation time of 30 seconds.
Further, the substrate is conductive glass deposited with titanium oxide.
Further, the vacuum drying gas in the step (4) is one or a mixture of more than one of argon, nitrogen and oxygen.
The perovskite thin film prepared by the preparation method of the perovskite thin film is applied to the preparation of solar cells, light-emitting diodes, photosensitive diodes, lasers, thin film transistors, photoelectric detectors or microsensors.
The invention has the beneficial effects that:
the invention relates to a preparation method and application of a perovskite film, which is characterized in that inorganic halogen salt containing bismuth, N-dimethylformamide solution, hydroiodic acid and raw materials are used for preparing the perovskite film with the general formula: DMABiIz1Brz2Cl3-z1-z2The intermediate material is used as a raw material, and the intermediate material and a lead-containing inorganic halogen salt, cesium iodide and an N, N-dimethylformamide solution are used as raw materials to prepare a precursor solution, wherein the lead-containing inorganic halogen salt can be pure lead iodide or a binary or ternary blend of lead iodide, lead chloride and lead bromide, one of the blends is lead iodide, and the general formula of the perovskite film prepared from the precursor solution is as follows: csxDMA1-xBiyPb1-yIz1Brz2Cl3-z1-z2，(x≠0、x≠1；y≠0、y is not equal to 1; z1 is not equal to 0, z2 is not equal to 0), the structure of the perovskite crystal is ABX3The perovskite film has three conditions of A site occupied by CS and DMA, B site occupied by Pb and Bi and X site occupied by I, Br, I, Cl or I, Br and Cl, and has good stability when subjected to stability test, and simultaneously, the photoelectric conversion rate can exceed 10 percent, and the black perovskite film can be obtained at the temperature of 80-150 ℃.
Drawings
FIG. 1 is a block diagram of a process for the preparation of perovskite membranes according to the present invention;
fig. 2 is a stability test chart of the perovskite films prepared in example one and comparative example 1.
Detailed Description
The technical solution of the present invention is further described with reference to the accompanying drawings 1-2 and the embodiments.
Example one
(1) Dissolving 2g of bismuth bromide in 5ml of N, N-dimethylformamide solution;
(2) dropwise adding 3ml of hydriodic acid after the bismuth bromide in the step (1) is dissolved, and stirring to obtain uniform light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2) and transferring the light yellow precipitate into a container to be washed by anhydrous ether so as to remove excessive hydroiodic acid and N, N-dimethylformamide solution;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven filled with argon at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
the intermediate material in this case has the general formula: DMABiBr3；
(5) Weighing 0.4g of the intermediate material in the step (4), weighing 0.32g of lead iodide and 0.2g of cesium iodide, and dissolving the three raw materials into 1ml of N, N-dimethylformamide solution to obtain a precursor solution;
the general formula of the precursor solution at this time is: cs0.7DMA0.3Bi0.3Pb0.7I2.1Br0.9；
(6) Coating the precursor solution in the step (5) on the conductive glass deposited with titanium oxide, and then placing the substrate in a spin coater, wherein the spin coater rotates for 30s at the rotating speed of 4000 revolutions per second;
(7) and (4) placing the substrate in the step (6) on a hot bench at 80 ℃ to carry out thermal annealing treatment for 5min so as to form the black perovskite film.
Example two
(1) Dissolving 1g of bismuth bromide and 1g of bismuth iodide in 5ml of N, N-dimethylformamide solution;
(2) dropwise adding 3ml of hydriodic acid after the bismuth bromide and the bismuth iodide in the step (1) are dissolved, and stirring to obtain uniform light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2) and transferring the light yellow precipitate into a container to be washed by anhydrous ether so as to remove excessive hydroiodic acid and N, N-dimethylformamide solution;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven filled with oxygen at 60 ℃ for 12 hours to obtain an intermediate material;
the intermediate material in this case has the general formula: DMABiI2.4Br0.6；
(6) Weighing 0.3g of the intermediate material in the step (4), weighing 0.37g of lead iodide and 0.2g of cesium iodide, and dissolving the three raw materials into 1ml of N, N-dimethylformamide solution to obtain a precursor solution;
the general formula of the precursor solution at this time is: cs0.8DMA0.2Bi0.2Pb0.8I2.4Br0.6；
(6) Coating the precursor solution in the step (5) on the conductive glass deposited with titanium oxide, and then placing the substrate in a spin coater, wherein the spin coater rotates for 30s at the rotating speed of 4000 revolutions per second;
(7) and (4) placing the substrate in the step (6) on a hot bench at 100 ℃ to carry out thermal annealing treatment for 5min so as to form the black perovskite film.
EXAMPLE III
(1) Dissolving 1g of bismuth chloride and 1g of bismuth iodide in 8ml of N, N-dimethylformamide solution;
(2) after the bismuth bromide and the bismuth iodide in the step (1) are dissolved, dropwise adding 5ml of hydriodic acid, and stirring to obtain uniform light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2) and transferring the light yellow precipitate into a container to be washed by anhydrous ether so as to remove excessive hydroiodic acid and N, N-dimethylformamide solution;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven filled with argon, nitrogen and oxygen at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
in this case the intermediate material has the general formula DMABiI2.9Cl0.1；
(7) Weighing 0.5g of the intermediate material in the step (4), weighing 0.27g of lead iodide, 0.03g of lead chloride and 0.2g of cesium iodide, and dissolving the three raw materials into 1ml of N, N-dimethylformamide solution to obtain a precursor solution;
the general formula of the precursor solution at this time is: cs0.8DMA0.2Bi0.4Pb0.6I2.9Cl0.1；
(6) Coating the precursor solution in the step (5) on the conductive glass deposited with titanium oxide, and then placing the substrate in a spin coater, wherein the spin coater rotates for 30s at the rotating speed of 4000 revolutions per second;
(7) and (4) placing the substrate in the step (6) on a hot bench at 120 ℃ to carry out thermal annealing treatment for 5min so as to form the black perovskite film.
Example four
(1) Dissolving 2g of bismuth bromide, 1g of bismuth chloride and 1g of bismuth iodide in 10ml of N, N-dimethylformamide solution;
(2) after the bismuth bromide and the bismuth iodide in the step (1) are dissolved, dropwise adding 6ml of hydriodic acid, and stirring to obtain uniform light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2) and transferring the light yellow precipitate into a container to be washed by anhydrous ether so as to remove excessive hydroiodic acid and N, N-dimethylformamide solution;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven filled with argon at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
the intermediate material in this case has the general formula: DMABiI1.2Br0.9Cl0.9；
(8) Weighing 0.8g of the intermediate material in the step (4), weighing 0.8g of lead iodide, 0.1g of lead chloride, 0.1g of lead bromide and 0.2g of cesium iodide, and dissolving the three raw materials into 2ml of N, N-dimethylformamide solution to obtain a precursor solution;
the general formula of the precursor solution at this time is: cs0.8DMA0.2Bi0.6Pb0.4I1.2Br0.9Cl0.9；
(6) Coating the precursor solution in the step (5) on the conductive glass deposited with titanium oxide, and then placing the substrate in a spin coater, wherein the spin coater rotates for 30s at the rotating speed of 4000 revolutions per second;
(7) and (4) placing the substrate in the step (6) on a hot bench at 150 ℃ to carry out thermal annealing treatment for 5min so as to form the black perovskite film.
Comparative example 1
(1) Dissolving 2g of lead iodide in 5ml of N, N-dimethylformamide solution;
(2) after the lead iodide in the step (1) is dissolved, dropwise adding 3ml of hydriodic acid, and stirring to obtain a uniform light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2) and transferring the light yellow precipitate into a container to be washed by anhydrous ether so as to remove excessive hydroiodic acid and N, N-dimethylformamide solution;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven filled with argon at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
the intermediate material in this case has the general formula: DMAPbI3；
(9) Weighing 0.4g of the intermediate material in the step (4), weighing 0.2g of cesium iodide, and dissolving the three raw materials into 1ml of N, N-dimethylformamide solution to obtain a precursor solution;
the general formula of the precursor solution at this time is: cs0.8DMA0.2PbI3；
(6) Coating the precursor solution in the step (5) on the conductive glass deposited with titanium oxide, and then placing the substrate in a spin coater, wherein the spin coater rotates for 30s at the rotating speed of 4000 revolutions per second;
(7) placing the substrate in the step (6) on a hot bench at 200 ℃ to carry out thermal annealing treatment for 5min so as to form a black perovskite film;
the perovskite film can be applied to solar cells, light emitting diodes, photosensitive diodes, lasers, thin film transistors, photodetectors or microsensors.
Comparative example 2
(1) Dissolving 1.8g of lead iodide and 0.2g of lead chloride in 5ml of an N, N-dimethylformamide solution;
(2) after the lead iodide in the step (1) is dissolved, dropwise adding 3ml of hydriodic acid, and stirring to obtain a uniform light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2) and transferring the light yellow precipitate into a container to be washed by anhydrous ether so as to remove excessive hydroiodic acid and N, N-dimethylformamide solution;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven filled with argon at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
the intermediate material in this case has the general formula: DMAPbI2.3Cl0.7；
(10) Weighing 0.4g of the intermediate material in the step (4), weighing 0.2g of cesium iodide, and dissolving the three raw materials into 1ml of N, N-dimethylformamide solution to obtain a precursor solution;
the general formula of the precursor solution at this time is: cs0.8DMA0.2PbI2.3Cl0.7；
(6) Coating the precursor solution in the step (5) on the conductive glass deposited with titanium oxide, and then placing the substrate in a spin coater, wherein the spin coater rotates for 30s at the rotating speed of 4000 revolutions per second;
(7) placing the substrate in the step (6) on a hot bench at 200 ℃ to carry out thermal annealing treatment for 5min so as to form a black perovskite film;
the perovskite film can be applied to solar cells, light emitting diodes, photosensitive diodes, lasers, thin film transistors, photodetectors or microsensors.
Comparative example 3
(1) Dissolving 1.6g of lead iodide, 0.2g of lead chloride and 0.2g of lead bromide in 5ml of an N, N-dimethylformamide solution;
(2) after the lead iodide in the step (1) is dissolved, dropwise adding 3ml of hydriodic acid, and stirring to obtain a uniform light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2) and transferring the light yellow precipitate into a container to be washed by anhydrous ether so as to remove excessive hydroiodic acid and N, N-dimethylformamide solution;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven filled with argon at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
the intermediate material in this case has the general formula: DMAPbI0.8Br1.5Cl0.7；
(11) Weighing 0.4g of the intermediate material in the step (4), weighing 0.2g of cesium iodide, and dissolving the three raw materials into 1ml of N, N-dimethylformamide solution to obtain a precursor solution;
the chemical formula of the precursor solution is: cs0.8DMA0.2PbI0.8Br1.5Cl0.7；
(6) Coating the precursor solution in the step (5) on the conductive glass deposited with titanium oxide, and then placing the substrate in a spin coater, wherein the spin coater rotates for 30s at the rotating speed of 4000 revolutions per second;
(7) placing the substrate in the step (6) on a hot bench at 200 ℃ to carry out thermal annealing treatment for 5min so as to form a black perovskite film;
the perovskite films prepared in the first, second, third and fourth embodiments can be applied to solar cells, light emitting diodes, photodiodes, lasers, thin film transistors, photodetectors or microsensors, and the photoelectric conversion efficiency is over 10%, the light conversion efficiency is over 10% in the comparative examples 1 and 2 but the stability is poor, and the light conversion efficiency is 6% in the comparative example 3 and the stability is also poor.
The invention introduces bismuth element into B site of perovskite crystal structure, and takes bismuth-containing inorganic halogen salt as one of raw materials to prepare bismuth-containing DMABiIz1Brz2Cl3-z1-z2And then taking the intermediate material as one of the raw materials, and adding lead-containing inorganic halogen and other raw material salts to prepare the intermediate material, wherein the intermediate material simultaneously comprises the following components: csxDMA1-xBiyPb1- yIz1Brz2Cl3-z1-z2And (x is not equal to 0, x is not equal to 1, y is not equal to 0, y is not equal to 1, z1 is not equal to 0, z2 is not equal to 0), finally, the precursor solution is deposited on the conductive glass attached with the titanium oxide by adopting a spin coater mode, and thermal annealing treatment is carried out at the temperature of 80-150 ℃ to finally obtain the perovskite film with the photoelectric conversion efficiency of more than 8% and good stability, wherein both the A site and the B site in the perovskite crystal structure are occupied by two ions, the tolerance factor of the crystal is improved, the stability of the perovskite film is better, and meanwhile, the photoelectric conversion efficiency can also exceed 8%.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.

Claims (9)

1. A method for preparing a perovskite film is characterized by comprising the following steps:
(1) dissolving inorganic halogen salt containing bismuth in N, N-dimethylformamide solution;
(2) dropwise adding hydroiodic acid after the bismuth-containing inorganic halogen salt in the step (1) is dissolved, and stirring to obtain a light yellow precipitate;
(3) vacuum filtering the light yellow precipitate in the step (2), transferring the light yellow precipitate into a container, and washing the light yellow precipitate with anhydrous ether;
(4) transferring the light yellow precipitate washed in the step (3) into a container again, and drying the container in a vacuum drying oven at the temperature of 60 ℃ for 12 hours to obtain an intermediate material;
(5) weighing the intermediate material in the step (4), weighing lead-containing inorganic halogen salt and cesium iodide, and dissolving all the raw materials into an N, N-dimethylformamide solution to obtain a precursor solution;
(6) depositing the precursor solution in the step (5) on a substrate;
(7) carrying out thermal annealing treatment on the substrate in the step (6) to form a black perovskite film;
wherein the inorganic halogen salt containing bismuth is one or a mixture of more than one of bismuth iodide, bismuth chloride and bismuth bromide;
the lead-containing inorganic halogen salt is lead iodide or a mixture of more than one of lead iodide, lead chloride and lead bromide, and one of the mixtures is lead iodide;
the intermediate material has the general formula: DMABiIz1Brz2Cl3-z1-z2；
The general formula of the precursor solution is as follows: csxDMA1-xBiyPb1-yIz1Brz2Cl3-z1-z2，(x≠0、x≠1；y≠0、y≠1；z1≠0、z2≠0)。
2. The method of claim 1, wherein the bismuth-containing inorganic halogen salt is bismuth bromide and the lead-containing inorganic halogen salt is lead iodide.
3. The method for producing a perovskite film as claimed in claim 1, wherein the thermal annealing treatment temperature in the step (7) is 80 ℃ to 150 ℃ and the annealing time is 5 min.
4. The method for preparing a perovskite film as claimed in claim 1, wherein the mass ratio of the precursor material, the lead-containing inorganic halogen salt and the cesium iodide in the step (5) is (1.5-2.5): (2-2.5): (0.5 to 1).
5. The method of claim 1, wherein the mass of lead iodide in the mixture of lead-containing inorganic halogen salts in step (1) is 80-90% of the total mass of the mixture.
6. The method of claim 1, wherein in step (6), the precursor solution is deposited on the substrate by using a spin coater at 4000 rpm for 30 seconds.
7. The method of claim 1, wherein the substrate is a conductive glass deposited with titanium oxide.
8. The method for preparing a perovskite film as claimed in claim 1, wherein the vacuum drying gas in step (4) is one or more of argon, nitrogen and oxygen.
9. The perovskite thin film prepared by the perovskite thin film preparation method as claimed in any one of claims 1 to 8 is applied to the preparation of solar cells, light emitting diodes, photodiodes, lasers, thin film transistors, photodetectors or microsensors.
CN202111517985.1A 2021-12-13 2021-12-13 Preparation method and application of perovskite film Pending CN114203906A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023184620A1 (en) * 2022-04-01 2023-10-05 暨南大学 Perovskite material and application thereof in solar cell

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023184620A1 (en) * 2022-04-01 2023-10-05 暨南大学 Perovskite material and application thereof in solar cell

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