CN115491201A - Preparation method of halide perovskite thin film with controllable thickness - Google Patents

Preparation method of halide perovskite thin film with controllable thickness Download PDF

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CN115491201A
CN115491201A CN202211055488.9A CN202211055488A CN115491201A CN 115491201 A CN115491201 A CN 115491201A CN 202211055488 A CN202211055488 A CN 202211055488A CN 115491201 A CN115491201 A CN 115491201A
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halide perovskite
thin film
crystal grains
halide
coating
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任天令
囤冠华
覃肯
耿祥顺
谢丹
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Tsinghua University
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
    • C09K11/7428—Halogenides
    • C09K11/7435—Halogenides with alkali or alkaline earth metals
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Abstract

The invention discloses a preparation method of a halide perovskite thin film with controllable thickness, which comprises the following steps: preparing halide perovskite crystal grains; mixing the halide perovskite crystal grains with a solvent and an additive to form slurry; coating the slurry on a substrate, heating, and repeating the coating and heating steps to obtain a halide perovskite thin film with controllable thickness; wherein the number of repetitions is equal to or greater than 0. Therefore, the method can reduce the internal defects of gaps, inversion and the like of crystal grains and improve the quality of the halide perovskite film. Meanwhile, the thickness of the halide perovskite thin film can be controlled by controlling the repeated times of the coating and heating steps, the thickness of the halide perovskite thin film can be adjusted from hundreds of nanometers to several centimeters, the requirements of different scenes can be met, and the defect that the halide perovskite thin film with larger thickness is difficult to prepare by the traditional method is overcome.

Description

Preparation method of halide perovskite thin film with controllable thickness
Technical Field
The invention belongs to the technical field of photoelectric materials, and particularly relates to a preparation method of a halide perovskite thin film with controllable thickness.
Background
Halide perovskites are very suitable for being used as semiconductor active layer materials in solar cells, light emitting diodes, lasers, photoelectric detectors and X-ray detectors due to the characteristics of excellent optical/X-ray absorption coefficient, long carrier life, high defect tolerance, low-temperature process and the like. In the application of X-ray detection, the perovskite film is required to have higher thickness (dozens of micrometers to several millimeters) due to the strong penetration characteristic of X-rays, and meanwhile, the development of a thickness-adjustable perovskite film preparation method is of great significance in consideration of the antagonistic trend between X-ray absorption and carrier transport between different thicknesses (the absorption is more sufficient in the case of high thickness, but the carrier is not easily transmitted, and the carrier is easily transmitted in the case of low thickness, but the absorption is insufficient). However, current methods of spin coating, blade coating, and the like still face challenges in preparing thin films with thicknesses greater than several tens of micrometers, while a large number of defects are present in the perovskite film due to volatilization of the solvent, and are subject to the temperature resistance of the substrate, which defects are difficult to eliminate by annealing, and the like.
Therefore, there is a need for improved methods for preparing halide perovskite thin films.
Disclosure of Invention
The present invention is made based on the discovery and recognition of the following facts and problems by the inventors.
The inventors have found that perovskite films obtained by conventional halide perovskite thin film preparation methods such as spin coating, spray coating, printing and the like mainly comprise two steps of deposition of a liquid precursor solution in which perovskite is dissolved, and subsequent drying to form a film. The quality and thickness controllability of the perovskite films prepared by these methods need to be improved. First, a number of defects are introduced during the manufacturing process. With the volatilization of the precursor solution solvent, the perovskite quickly nucleates and grows on the substrate. The fast growth rate results in the formation of a large number of internal defects. Solvent evaporation and perovskite nucleation growth preferentially occur on the liquid surface, which results in the formation of a solid 'shell' on the outermost layer, and the 'shell' can be broken when the internal solvent is evaporated, so that a large number of surface defects are introduced. In view of the temperature tolerance of the substrate (such as a thin film transistor array), it is not possible to reduce the defect density by means of high temperature annealing or the like. Secondly, due to the fluidity and surface tension of the perovskite precursor solution, the thickness of the liquid film cannot be effectively controlled, and a film of several tens to several hundreds of micrometers cannot be obtained.
The present invention aims to ameliorate at least one of the above technical problems to at least some extent.
The invention provides a preparation method of a halide perovskite thin film with controllable thickness, which comprises the following steps:
preparing halide perovskite crystal grains;
mixing the halide perovskite crystal grains with a solvent and an additive to form slurry;
coating the slurry on a substrate, heating, and repeating the coating and heating steps to obtain a halide perovskite thin film with controllable thickness;
wherein the number of repetitions is equal to or greater than 0.
Therefore, the method can reduce internal defects such as gaps and inversion of crystal grains and improve the quality of the halide perovskite thin film. Meanwhile, the thickness of the halide perovskite thin film can be controlled by controlling the repeated times of the coating and heating steps, the thickness of the halide perovskite thin film can be adjusted from hundreds of nanometers to several centimeters, the requirements of different scenes can be met, and the defect that the halide perovskite thin film with larger thickness is difficult to prepare by the traditional method is overcome.
According to an embodiment of the invention, the halide perovskite has the chemical formula Cs 2 AgBiBr 6 Or A 3 B 2 X 9 Wherein A is Cs or NH 4 、CH 3 NH 3 B is Bi, and X is at least one of Cl, br and I.
According to an embodiment of the present invention, when the halide perovskite has the chemical formula Cs 2 AgBiBr 6 In this regard, preparing the halide perovskite grains includes: csBr, agBr, biBr 3 Mixing with dimethyl sulfoxide, reacting at 110-130 deg.C 2Obtaining halide perovskite precursor solution after 5-3.5 h; and adding isopropanol into the halide perovskite precursor solution to obtain a suspension, and filtering the suspension to obtain halide perovskite crystal grains.
According to an embodiment of the present invention, when the halide perovskite has the formula A 3 B 2 X 9 In this regard, preparing the halide perovskite grains includes: mixing AX and BX 3 Mixing with HX, and reacting at 110-130 ℃ for 2.5-3.5 h to obtain halide perovskite precursor solution; and reducing the temperature of the halide perovskite precursor solution to room temperature to obtain halide perovskite crystal grains.
According to an embodiment of the invention, when the halide perovskite has the chemical formula Cs 2 AgBiBr 6 After preparing the halide perovskite grains, the method further comprises: carrying out air annealing treatment on the halide perovskite crystal grains; and then mixing the halide perovskite crystal grains subjected to the air annealing treatment with a solvent and an additive to form slurry. Therefore, internal defects such as gaps and inversion of crystal grains can be effectively reduced through annealing treatment, unsaturated dangling bonds on the surface are passivated, and the quality of the halide perovskite film is further improved.
According to the embodiment of the invention, the temperature of the air annealing treatment is 250-300 ℃, and the time of the air annealing treatment is 5-10 min. Thus, by performing the air annealing treatment under the above-described conditions, the density of defects such as dislocations in crystal grains can be more effectively reduced, and the quality of the halide perovskite thin film can be improved.
According to an embodiment of the present invention, the solvent includes at least one of terpineol and isopropyl alcohol, and the additive includes at least one of polyimide and polyvinyl alcohol.
According to the embodiment of the invention, the mass percentage of the additive to the halide perovskite crystal grains is 1-10%.
According to the embodiment of the invention, the substrate comprises a base material layer and a transition layer which are arranged in a laminated mode, wherein the base material layer is a thin film transistor array or a complementary metal oxide transistor array; the slurry is coated on the transition layer; the coating mode is blade coating, and the distance between a blade and the substrate is more than or equal to 5 mu m; for example, the distance between the blade and the substrate is 100 μm or 500 μm.
According to the embodiment of the invention, the heating temperature is 40-60 ℃; the heating time is 0.5-1.5 h. By heating, the solvent can be removed to form a dense halide perovskite thin film.
Drawings
FIG. 1 is a flow chart of a method of preparing a controlled thickness halide perovskite thin film in accordance with the present invention;
FIG. 2 shows Cs prepared by conventional knife coating 2 AgBiBr 6 A time-resolved photoluminescence spectrum of a halide perovskite thin film;
FIG. 3 is Cs prepared in example 1 2 AgBiBr 6 A time-resolved photoluminescence spectrum of a halide perovskite thin film;
FIG. 4 is a scanning electron micrograph of a halide perovskite thin film prepared in example 1, in which the number of coating and heating was 1;
FIG. 5 is a scanning electron micrograph of a halide perovskite thin film prepared in example 1, in which the coating and heating were repeated 3 times;
FIG. 6 is a scanning electron micrograph of the halide perovskite thin film prepared in example 2.
Detailed Description
Embodiments of the present application are described in detail below. The following description of the embodiments is merely exemplary in nature and is in no way intended to limit the present disclosure. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents used are conventional products which are commercially available, not indicated by the manufacturer.
The invention provides a preparation method of a halide perovskite thin film with controllable thickness, and with reference to figure 1, the method comprises the following steps:
s100, preparing halide perovskite crystal grains;
the chemical formula of the halide perovskite is Cs 2 AgBiBr 6 Or A 3 B 2 X 9 Wherein A is Cs or NH 4 、CH 3 NH 3 B is Bi, and X is at least one of Cl, br and I.
When the chemical formula of the halide perovskite is Cs 2 AgBiBr 6 In this regard, preparing the halide perovskite grains includes:
CsBr, agBr, biBr 3 Mixing with dimethyl sulfoxide, and reacting at 110-130 deg.C (such as 110 deg.C, 115 deg.C, 120 deg.C, 125 deg.C, 130 deg.C) for 2.5-3.5 h (such as 2.5h, 3h, 3.5 h) to obtain halide perovskite precursor solution;
and adding isopropanol into the halide perovskite precursor solution to obtain a suspension, and filtering the suspension to obtain halide perovskite crystal grains.
When the chemical formula of the halide perovskite is Cs 2 AgBiBr 6 After preparing the halide perovskite grains, the method further comprises: carrying out air annealing treatment on the halide perovskite crystal grains; and then mixing the halide perovskite crystal grains subjected to air annealing treatment with a solvent and an additive to form slurry.
According to some embodiments of the invention, the temperature of the air annealing treatment is 250-300 ℃, such as 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 300 ℃, and the time of the air annealing treatment is 5-10 min, such as 5min, 6min, 7min, 8min, 9min, 10min. Through air annealing treatment, the internal defect state density of gaps, inversion positions and the like of crystal grains can be reduced, and unsaturated dangling bonds on the surface are passivated. Because the crystal grains are not contacted with the substrate when being annealed, the annealing temperature is not limited by the temperature endured by the substrate, namely the annealing treatment of the invention can not cause adverse effect on the substrate. Under the air annealing treatment condition, the quality of the halide perovskite film is further improved.
According to some embodiments of the invention, the thickness of the halide perovskite thin film may be controlled by controlling the size of the halide perovskite grains.
According to some embodiments of the invention, when the halide perovskite has the formula a 3 B 2 X 9 In this regard, preparing the halide perovskite grains includes:
mixing AX and BX 3 Mixing with HX, and reacting at 110-130 deg.C (such as 110 deg.C, 115 deg.C, 120 deg.C, 125 deg.C, 130 deg.C) for 2.5-3.5 h (such as 2.5h, 3h, 3.5 h) to obtain halide perovskite precursor solution;
and reducing the temperature of the halide perovskite precursor solution to room temperature to obtain halide perovskite crystal grains.
S200, mixing halide perovskite crystal particles with a solvent and an additive to form slurry;
the solvent comprises at least one of terpineol and isopropanol, and the additive comprises at least one of polyimide and polyvinyl alcohol. The halide perovskite crystal particles are insoluble in the solvent and the additive, and the resulting slurry is a suspension. The purpose of the solvent is to disperse the halide perovskite grains to form a suspension, which facilitates the transfer of the halide perovskite grains to the substrate.
The mass percentage of the additive to the halide perovskite crystal grains is 1% to 10%, for example, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.
In some embodiments of the invention, the ratio of the mass of the solvent to the mass of the halide perovskite grains is 1.
According to some embodiments of the present invention, the thickness of the halide perovskite thin film may be controlled by controlling the concentration of the slurry.
S300, coating the slurry on a substrate, heating, and repeating the coating and heating steps to obtain a halide perovskite thin film with controllable thickness;
wherein the number of repetitions is equal to or greater than 0. Assuming that the number of repetitions is n, n +1 coating steps, n +1 heating steps are required on the substrate. When n is 0, the halide perovskite thin film can be formed by performing a coating step and a heating step on the substrate.
The substrate comprises a base material layer and a transition layer which are arranged in a stacked mode, wherein the base material layer is a thin film transistor array or a complementary metal oxide transistor array (CMOS); the material for forming the transition layer comprises polyimide and Cs 3 Bi 2 Y 9 Mixture of perovskites, cs 3 Bi 2 Y 9 The mass fraction of perovskite in the mixture is 50%, wherein Y is selected from Br or I. The slurry is coated on the transition layer.
In some embodiments of the present invention, the coating is blade coating, and the distance between the blade and the substrate is greater than or equal to 5 μm, for example, 5 μm, 10 μm, 50 μm, 100 μm, 500 μm; the thickness of the halide perovskite thin film can be controlled by adjusting the distance between the scraper and the substrate.
The coating method in the present invention is not limited to blade coating, and may be other methods such as spray coating.
The halide perovskite thin film may be transferred to a substrate by a coating step resulting in an integrated device.
The thickness of the halide perovskite thin film can be controlled by adjusting the repeated times of the coating and heating steps, and the halide perovskite thin film with controllable thickness is obtained.
According to some embodiments of the invention, the temperature of the heating is 40 to 60 ℃, e.g. 40 ℃, 45 ℃, 50 ℃, 55 ℃,60 ℃; the heating time is 0.5-1.5 h, such as 0.5h, 1h, 1.5h. Under the heating condition, the solvent can be removed to obtain a dense halide perovskite thin film.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way. In the following examples and comparative examples, the reagents used were, unless otherwise specified, commercially available analytical grade products.
Example 1
1. Grain preparation
Taking 10mmol CsBr, 5mmol AgBr and 5mmolBiBr 3 And adding 10mL of dimethyl sulfoxide (DMSO) into the powder, and heating for 3h at 120 ℃ until the solution is completely clear to obtain a perovskite precursor solution.
And taking 500 mu L of perovskite precursor solution by using a liquid transfer gun, and slowly dripping the solution into 10mL of isopropanol solvent under the condition of vigorous stirring to obtain orange-red suspension.
Filtering the orange-red suspension by adopting a low-pressure filtering method to obtain perovskite crystal grains, and washing the perovskite crystal grains with isopropanol for 2-3 times. The rinsed grains were air annealed at 280 ℃ for 5min. The grain size obtained is in the range of 1 μm to 10 μm.
1g of the crystal grains were dispersed in 1g of terpineol, 0.01g of polyvinyl alcohol was added thereto, and the mixture was sufficiently stirred to form a suspension slurry.
2. Knife coating deposition
A layer of polyimide/Cs (100-2000rpm, 30s) is spin-coated on thin film transistor arrays (TFTs) 3 Bi 2 Br 9 Perovskite (perovskite mass fraction is 50%) is regarded as the transition layer, 60 ℃ dries for 30min and obtains the required substrate of blade coating.
And depositing the perovskite slurry on the prepared substrate by adopting a scraper coating method, controlling the distance between the scraper and the substrate to be about 100 mu m, heating at the low temperature of 50 ℃ for 1h to completely volatilize terpineol, and obtaining a perovskite film with the thickness of about 100 mu m according to a picture 4. The coating, heating step was repeated 3 times, see fig. 5, resulting in a perovskite film having a thickness of about 400 μm.
FIGS. 2 and 3 show Cs prepared by the conventional knife coating method, respectively 2 AgBiBr 6 Halide perovskite thin film and Cs prepared in example 1 2 AgBiBr 6 Time-resolved photoluminescence spectrograms of the halide perovskite thin film are shown in fig. 2 and fig. 3, and compared with the traditional knife coating method, the fluorescence lifetime of the halide perovskite thin film obtained by the method is prolonged, which indicates that the quality of the halide perovskite thin film is improved.
Example 2
1. Grain preparation
1.5mmol CsBr and 1mmol BiBr are taken 3 Adding the powder into a 10mL 9mol/L HBr solution, and heating at 120 ℃ for 3h until the solution is completely clear to obtainCs 3 Bi 2 Br 9 A perovskite precursor solution.
Cooling to room temperature from 120 ℃ at the speed of 1 ℃/min to obtain the perovskite crystal grain with the grain diameter ranging from 10 mu m to 50 mu m.
1g of the crystal grains were dispersed in 1g of terpineol, 0.01g of polyimide was added thereto, and the mixture was sufficiently stirred to form a suspension slurry.
2. Knife coating deposition
A layer of polyimide/Cs (100-2000rpm, 30s) is spin-coated on a complementary metal oxide array (CMOS) 3 Bi 2 I 9 Perovskite (perovskite mass fraction is 50%) is regarded as the transition layer, 60 ℃ dries for 30min and obtains the required substrate of blade coating.
And depositing the perovskite slurry on the prepared substrate by adopting a scraper coating method, controlling the distance between the scraper and the substrate to be 500 mu m, heating at the low temperature of 50 ℃ for 1h to completely volatilize terpineol, and referring to figure 6, thus obtaining the perovskite film with the thickness of about 500 mu m.
In the description herein, reference to the description of the terms "one embodiment," "another embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
While embodiments of the present application have been shown and described above, it will be understood that the above embodiments are exemplary and should not be construed as limiting the present application and that changes, modifications, substitutions and alterations in the above embodiments may be made by those of ordinary skill in the art within the scope of the present application.

Claims (10)

1. A method of making a halide perovskite thin film of controlled thickness, the method comprising:
preparing halide perovskite crystal grains;
mixing the halide perovskite crystal grains with a solvent and an additive to form slurry;
coating the slurry on a substrate, heating, and repeating the coating and heating steps to obtain a halide perovskite thin film with controllable thickness;
wherein the number of repetitions is equal to or greater than 0.
2. The production method according to claim 1, wherein the halide perovskite has a chemical formula of Cs 2 AgBiBr 6 Or A 3 B 2 X 9 Wherein A is Cs or NH 4 、CH 3 NH 3 B is Bi, and X is at least one of Cl, br and I.
3. The production method according to claim 2, wherein when the halide perovskite has a chemical formula of Cs 2 AgBiBr 6 In this regard, preparing the halide perovskite grains includes:
CsBr, agBr, biBr 3 Mixing the precursor solution with dimethyl sulfoxide, and reacting at 110-130 ℃ for 2.5-3.5 h to obtain a halide perovskite precursor solution;
and adding isopropanol into the halide perovskite precursor solution to obtain a suspension, and filtering the suspension to obtain halide perovskite crystal grains.
4. The production method according to claim 2, wherein when the halide perovskite has a chemical formula of A 3 B 2 X 9 In this case, preparing the halide perovskite grains includes:
mixing AX and BX 3 Mixing with HX, reacting at 110-130 deg.C for 2.5-3.5 h to obtain halide perovskiteA bulk solution;
and reducing the temperature of the halide perovskite precursor solution to room temperature to obtain halide perovskite crystal grains.
5. The production method according to claim 2, wherein when the halide perovskite has a chemical formula of Cs 2 AgBiBr 6 After preparing the halide perovskite grains, the method further comprises: carrying out air annealing treatment on the halide perovskite crystal grains; and then mixing the halide perovskite crystal grains subjected to air annealing treatment with a solvent and an additive to form slurry.
6. The method according to claim 5, wherein the temperature of the air annealing treatment is 250 to 300 ℃, and the time of the air annealing treatment is 5 to 10min.
7. The method according to claim 1, wherein the solvent includes at least one of terpineol and isopropyl alcohol, and the additive includes at least one of polyimide and polyvinyl alcohol.
8. The production method according to claim 1, wherein the mass percentage of the additive to the halide perovskite crystal grains is 1% to 10%.
9. The preparation method of claim 1, wherein the substrate comprises a base material layer and a transition layer which are stacked, and the base material layer is a thin film transistor array or a complementary metal oxide transistor array;
the slurry is coated on the transition layer;
optionally, the coating mode is blade coating, and the distance between a blade and the substrate is more than or equal to 5 μm;
optionally, the distance between the doctor blade and the substrate is 100 μm or 500 μm.
10. The method according to claim 1, wherein the heating temperature is 40 to 60 ℃;
the heating time is 0.5-1.5 h.
CN202211055488.9A 2022-08-29 2022-08-29 Preparation method of halide perovskite thin film with controllable thickness Pending CN115491201A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108329912A (en) * 2018-01-18 2018-07-27 华中科技大学 A method of improving the fluorescent yield and stability of non-lead halogen perovskite material
CN109817812A (en) * 2019-01-08 2019-05-28 武汉大学 Bulky grain perovskite monocrystalline/polymer composite thick film, photodetector and preparation method
CN110484246A (en) * 2019-08-20 2019-11-22 华中科技大学 A kind of double-perovskite nanocrystalline material is preparing the application in inorganic white light LED
CN110911566A (en) * 2019-12-06 2020-03-24 武汉大学 Perovskite single crystal particle composite film based X-ray detector and preparation method thereof
CN114420840A (en) * 2021-12-07 2022-04-29 清华大学 Patterned halogen perovskite thin film and preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108329912A (en) * 2018-01-18 2018-07-27 华中科技大学 A method of improving the fluorescent yield and stability of non-lead halogen perovskite material
CN109817812A (en) * 2019-01-08 2019-05-28 武汉大学 Bulky grain perovskite monocrystalline/polymer composite thick film, photodetector and preparation method
CN110484246A (en) * 2019-08-20 2019-11-22 华中科技大学 A kind of double-perovskite nanocrystalline material is preparing the application in inorganic white light LED
CN110911566A (en) * 2019-12-06 2020-03-24 武汉大学 Perovskite single crystal particle composite film based X-ray detector and preparation method thereof
CN114420840A (en) * 2021-12-07 2022-04-29 清华大学 Patterned halogen perovskite thin film and preparation method and application thereof

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