CN113410398A - Method for preparing perovskite photoelectric detector by anti-solvent one-step method - Google Patents
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Abstract
The invention provides a method for preparing a perovskite photoelectric detector by an anti-solvent one-step method. The detector prepared by the invention has the optical power density of 6.37 mu W/cm2Under the condition of irradiating the 532nm laser diode and biasing at-2V, the responsivity reaches 1.56A/W and the detectivity reaches 1.47 multiplied by 1012Jones, linear dynamic range reaches 110 dB. In addition, compared with the traditional anti-solvent, the tert-amyl alcohol has low manufacturing cost and is not controlled by hazardous chemicals, and reference is provided for preparing the high-performance vertical-structure perovskite photoelectric detector.
Description
Technical Field
The invention relates to the field of photoelectron materials and devices, in particular to a method for preparing a perovskite photoelectric detector by using an anti-solvent one-step method.
Background
The photoelectric detector can convert a light signal which is difficult to quantify into an electric signal which can be accurately detected, and plays a great role in industrial and scientific research, such as imaging, optical communication, chemical/biological sensing, environmental monitoring and the like. For photodetectors, the most important is the semiconductor material. The semiconductor material acts as a photoactive layer, capable of absorbing photon energy and generating photogenerated carriers (electron-hole pairs). These separated electrons and holes are transported to both ends of the electrode under the action of an internal electric field or an external bias voltage to generate a current signal. Currently, the commercial detectors mainly use inorganic semiconductor materials, such as GaN, Si, and InGaAs. The detectors have the advantages of mature preparation industry, clear working mechanism and the like, but the preparation processes are complex and expensive, and the driving voltage is high, so that the application range of the detectors is limited. Over the past decade or so, low-cost, solution-processable photovoltaic materials, such as organic materials, nanomaterials and nanocomposites, have shown great potential for application in the field of flexible large area detectors. However, these materials also have some considerable disadvantages, which have influenced their further development. Recently, perovskite materials have been widely used in solar cell, LED, laser and photodetector research due to their unique advantages of high carrier mobility, high light absorption coefficient, long carrier diffusion length, adjustable direct band gap, etc. The vertical-structure photoelectric detector has the advantages of short carrier transmission distance, fast frequency response, linear correlation between photocurrent and incident light intensity and the like, so that the vertical-structure photoelectric detector is very suitable for the fields of visible light communication and imaging.
The most important factors that have been reported to affect the performance of perovskite detectors are poor film quality and defects present at the surface and grain boundaries of the perovskite film. Therefore, it is important to find a way to effectively enhance the quality of the film. In order to better regulate the film-forming quality of the film, a very useful way is to add an anti-solvent, such as toluene, chlorobenzene, and other mixed anti-solvents, etc. dropwise in the perovskite spin-coating process, so that the perovskite nucleation and crystal growth processes can be effectively regulated, and the uniform, compact and pore-free perovskite film can be obtained. The anti-solvent used in the method is tert-amyl alcohol, and compared with the traditional anti-solvents, the tert-amyl alcohol serving as the anti-solvent has the advantages of better device performance, low toxicity, low cost, easiness in obtaining and the like, so that the method has more advantages compared with the traditional anti-solvents.
Disclosure of Invention
The invention provides a method for preparing a perovskite photoelectric detector by an anti-solvent one-step method, overcomes the defects of strong toxicity of the traditional anti-solvent, controlled solvent, difficult obtainment and the like, and obtains the device performance superior to the device performance of the traditional anti-solvent participating in preparation.
The technical scheme for realizing the invention is as follows:
the perovskite photoelectric detector comprises a conductive substrate, a hole transport layer, a perovskite thin film, an electron transport layer and a metal electrode, wherein the perovskite thin film is prepared by using an anti-solvent.
The anti-solvent is tert-amyl alcohol.
Preferably, the transparent conductive substrate can be ITO conductive glass, and can also be FTO or AZO, TCO.
Preferably, the hole transport layer is PEDOT PSS.
Preferably, the electron transport layer is PC61BM and BCP.
Preferably, the metal electrode may be gold, silver.
The optical power density of the perovskite photoelectric detector is 6.37 mu W/cm2Under the condition of irradiating the 532nm laser diode and biasing at-2V, the responsivity reaches 1.56A/W and the detectivity reaches 1.47 multiplied by 1012Jones, linear dynamic range reaches 110 dB.
The perovskite thin film is prepared by the following specific steps:
s1: preparing a perovskite precursor solution;
s2: dropwise adding a tert-amyl alcohol anti-solvent in the spin coating process of the perovskite precursor solution;
s3: and carrying out thermal annealing and solvent annealing treatment in sequence to obtain the perovskite thin film.
The perovskite in step S1 is CH3NH3PbI3。
The volume ratio of the perovskite precursor solution to the tertiary amyl alcohol antisolvent in the step S2 is 1 (2-3), and the perovskite precursor solution is spin-coated at 6000rpm for 30-60S.
And (S2) pre-annealing for 10-15S on a heating table after the spin coating is finished, taking out the sample, heating and annealing under the ambient air condition, and then continuously annealing for 10 minutes in a DMSO atmosphere to obtain the perovskite thin film.
The pre-annealing is carried out in a glove box protected by nitrogen, and the heating annealing temperature in the ambient air is 80-100 ℃ and the time is 10-30 min.
The invention has the beneficial effects that: the detector prepared by the invention has the optical power density of 6.37 mu W/cm2Under the condition of irradiating the 532nm laser diode and biasing at-2V, the responsivity reaches 1.56A/W and the detectivity reaches 1.47 multiplied by 1012Jones, linear dynamic range reaches 110 dB. In addition, compared with the traditional anti-solvent, the tert-amyl alcohol has low manufacturing cost and is not controlled by hazardous chemicals, and reference is provided for preparing the high-performance vertical-structure perovskite photoelectric detector.
The tert-amyl alcohol anti-solvent adopted by the invention has moderate polarity, and can effectively remove redundant DMF and DMSO solvent in the precursor solution in the dropping process, thereby accelerating homogeneous nucleation of perovskite and growth of perovskite crystal grains, and then obtaining a uniform, compact and pore-free high-quality perovskite thin film through high-temperature annealing and solvent annealing processes, thereby obtaining a high-performance vertical structure photoelectric detector.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the device structure of a perovskite photodetector.
FIG. 2 is a flow chart of perovskite thin film preparation using t-amyl alcohol as an anti-solvent.
FIG. 3 is an XRD pattern of a perovskite thin film prepared using t-amyl alcohol as an anti-solvent.
FIG. 4 is a scanning electron micrograph of a perovskite thin film prepared using t-amyl alcohol as an anti-solvent.
FIG. 5 is a graph of the responsivity of a perovskite photodetector fabricated using t-amyl alcohol as an anti-solvent.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
As shown in fig. 1, the device structure of the perovskite photodetector includes: the ITO conductive substrate, the hole transport layer, the perovskite thin film, the electron transport layer and the metal electrode.
Further, the transparent conductive substrate may be ITO conductive glass.
And furthermore, the hole transport layer is PEDOT PSS.
Further, the electron transport layer is PC61BM and BCP.
Further, the metal electrode may be gold or silver.
Example 1
Weighing a mixture with a molar ratio of 1: 1.05 CH3NH3I powder and PbI2Dissolving the powder in 1ml of mixed solvent of DMF (dimethylformamide) and DMSO (dimethyl sulfoxide) (the volume ratio of DMF to DMSO is 9:1), adding magnetons into the prepared solution, stirring for 12 hours, and reacting fully to obtain a clear yellowish perovskite precursor solution.
100 μ L of the precursor solution was dropped onto the substrate and spun at 6000rpm for 30 s. And (3) dropwise adding 250 mu L of anti-solvent tert-amyl alcohol in the spin coating process in the second step, and pre-annealing on a heating table for 10-15 s after the spin coating is finished, wherein the processes are carried out in a glove box protected by nitrogen. And taking out the sample, heating and annealing at 100 ℃ for 20 minutes under the ambient air condition, and then placing the sample in a DMSO atmosphere to continue annealing for 10 minutes to obtain the perovskite thin film.
As shown in an XRD diagram in FIG. 3, the perovskite thin film prepared by the one-step method by using tertiary amyl alcohol as an anti-solvent has obvious diffraction characteristic peaks at 14.1 degrees, 28.5 degrees and 31.9 degrees, which respectively correspond to 110, 220 and 310 crystal planes of perovskite crystals, and the perovskite thin film is formed, and the result is further proved by an SEM diagram in FIG. 4, and the uniform, dense and pore-free high-quality perovskite thin film is formed.
The preparation process of the perovskite photoelectric detector comprises the following steps: and (3) carrying out ultrasonic treatment on the ITO substrate by using a glass cleaning agent, deionized water, acetone and isopropanol in sequence, and then carrying out ultraviolet ozone treatment for 15 minutes. PSS (PEDOT) is added dropwise on the substrate, and spin coating is carried out at 4000rpm for 40 s. The perovskite thin film was then prepared according to the procedure described in example 1 above, followed by spin coating of PC in sequence61BM (4000rpm spin-on 40s) and BCP (6000rpm spin-on 40s), and finally 100nm Ag by thermal evaporation. The Responsivity (Responsivity) of the perovskite photodetector prepared by using tertiary amyl alcohol as an anti-solvent is 6.37 mu w/cm2The detection degree of the vertical structure perovskite photoelectric detector can reach 1.56A/W under the irradiation of a 532nm laser diode, the detection degree is shown in figure 5, and the detection degree (Detectivity) of the vertical structure perovskite photoelectric detector prepared by using tertiary amyl alcohol as an anti-solvent reaches 1.47 multiplied by 1012Jones, linear dynamic range reaches 110 dB. In addition, compared with the traditional anti-solvent, the tert-amyl alcohol has low manufacturing cost and is not controlled by hazardous chemicals, and reference is provided for preparing the high-performance vertical-structure perovskite photoelectric detector.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A method for preparing a perovskite photoelectric detector by an anti-solvent one-step method is characterized by comprising the following steps: the perovskite photoelectric detector comprises a conductive substrate, a hole transport layer, a perovskite thin film, an electron transport layer and a metal electrode, wherein the perovskite thin film is prepared by using an anti-solvent.
2. The method of claim 1, wherein: the anti-solvent is tert-amyl alcohol.
3. The method of claim 1, wherein: the optical power density of the perovskite photoelectric detector is 6.37 mu W/cm2Under the condition of irradiating the 532nm laser diode and biasing at-2V, the responsivity reaches 1.56A/W and the detectivity reaches 1.47 multiplied by 1012Jones, linear dynamic range reaches 110 dB.
4. The method according to any one of claims 1 to 3, wherein the perovskite thin film is prepared by the following specific steps:
s1: preparing a perovskite precursor solution;
s2: dropwise adding a tert-amyl alcohol anti-solvent in the spin coating process of the perovskite precursor solution;
s3: and carrying out thermal annealing and solvent annealing treatment in sequence to obtain the perovskite thin film.
5. The method of claim 4, wherein: the perovskite in the step S1 is CH3NH3PbI3。
6. The method of claim 4, wherein: the volume ratio of the perovskite precursor solution to the tertiary amyl alcohol antisolvent in the step S2 is 1 (2-3), and the perovskite precursor solution is spin-coated at 6000rpm for 30-60S.
7. The method of claim 4, wherein: and (S2) pre-annealing for 10-15S on a heating table after the spin coating is finished, taking out the sample, heating and annealing under the ambient air condition, and then continuously annealing for 10 minutes in a DMSO atmosphere to obtain the perovskite thin film.
8. The method of claim 7, wherein: and pre-annealing is carried out in a nitrogen-protected glove box, and the heating annealing temperature in the ambient air is 80-100 ℃ for 10-30 min.
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CN107359246A (en) * | 2017-06-20 | 2017-11-17 | 太原理工大学 | A kind of preparation method of methylamine lead iodine perovskite solar cell |
CN108217718A (en) * | 2018-03-13 | 2018-06-29 | 南方科技大学 | A kind of ABX3Nanocrystalline synthetic method of perovskite and products thereof and purposes |
CN111933807A (en) * | 2020-08-28 | 2020-11-13 | 电子科技大学 | High-stability perovskite photoelectric detector prepared based on additive treatment and preparation method thereof |
US20210166885A1 (en) * | 2018-08-09 | 2021-06-03 | Soochow University | Method for preparing inorganic perovskite battery based on synergistic effect of gradient annealing and antisolvent, and prepared inorganic perovskite battery |
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CN107359246A (en) * | 2017-06-20 | 2017-11-17 | 太原理工大学 | A kind of preparation method of methylamine lead iodine perovskite solar cell |
CN108217718A (en) * | 2018-03-13 | 2018-06-29 | 南方科技大学 | A kind of ABX3Nanocrystalline synthetic method of perovskite and products thereof and purposes |
US20210166885A1 (en) * | 2018-08-09 | 2021-06-03 | Soochow University | Method for preparing inorganic perovskite battery based on synergistic effect of gradient annealing and antisolvent, and prepared inorganic perovskite battery |
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