CN114530560A - Perovskite single crystal photoelectric detector and preparation method thereof - Google Patents

Perovskite single crystal photoelectric detector and preparation method thereof Download PDF

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CN114530560A
CN114530560A CN202210085136.1A CN202210085136A CN114530560A CN 114530560 A CN114530560 A CN 114530560A CN 202210085136 A CN202210085136 A CN 202210085136A CN 114530560 A CN114530560 A CN 114530560A
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single crystal
mapbcl
perovskite
mapbbr
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李林
闫珺
公维强
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Harbin Normal University
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
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Abstract

The invention discloses a perovskite single crystal photoelectric detector and a preparation method thereof, relating to the technical field of photoelectric detectors, wherein the preparation method of the perovskite single crystal photoelectric detector comprises the following steps: s1, preparing a perovskite precursor solution; s2, basic MAPbCl3Growing a single crystal; s3, heterogeneous MAPbCl3‑MAPbBr3Growing a single crystal; s4, preparing the perovskite single crystal photoelectric detector. The preparation method of the perovskite single crystal photoelectric detector provided by the invention is simple to operate, has stable technology, has no strict requirements on preparation environment, is easy to obtain raw materials, has excellent effect, can keep stable work in air environment, and solves the technical problem that the detector can work without connecting an external voltage. The perovskite single crystal photoelectric detector provided by the invention has the characteristic of self-driving, has higher spectral responsivity and environmental stability, and can be used for detecting long-term optical signals.

Description

Perovskite single crystal photoelectric detector and preparation method thereof
Technical Field
The invention relates to the technical field of photoelectric detectors, in particular to a perovskite single crystal photoelectric detector and a preparation method thereof.
Background
The photoelectric detector has the capability of converting optical signals into electric signals, and is widely applied to the fields of image sensing, optical communication, environment monitoring and the like. Most of the traditional photodetectors adopt inorganic semiconductor materials such as Si, SiC, InGaAs, GaN and the like, but the semiconductor materials need to grow in a high vacuum environment, and the preparation process is complex. And the traditional photoelectric detector can detect the optical signal only by being driven by an external power supply, so that the cost is increased, and the complexity of a test system is increased.
In the last decade, organic-inorganic hybrid perovskite materials have been widely used in many fields of optoelectronic devices, including photodetectors, lasers, solar cells, light emitting diodes, etc., due to their simple synthesis method and excellent optoelectronic properties, such as high absorption coefficient, long carrier diffusion length, high carrier mobility, low exciton binding energy, etc.
The perovskite polycrystalline thin film material is easy to degrade in an air environment due to the existence of crystal boundaries and pores, and is poor in stability. This problem has been a major obstacle to practical application of perovskite materials. Compared with a polycrystalline thin film, the perovskite Single Crystal (SC) has the advantages of low trap state density, good stability and the like. Because of these advantages, it is important to produce a high-performance and stable photodetector.
The self-powered detector has the advantages of small size, light weight, easiness in integration and the like, and can meet the requirements of extreme environment testing and portable equipment. The self-powered detector may be implemented by the photovoltaic effect of schottky junctions and heterojunctions. Most perovskite-based photodetectors in the prior art use essentially one perovskite material and another material to form a heterojunction device structure to achieve self-powered detection.
At present, no heterojunction device composed of two perovskite single crystal materials is used for realizing a self-powered perovskite single crystal photoelectric detector.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a perovskite single crystal photoelectric detector and a preparation method thereof.
On the one hand, the invention provides a preparation method of a perovskite single crystal photoelectric detector, which comprises the following steps:
s1, preparation of a perovskite precursor solution:
weighing MACl and PbCl2Adding the powder into a mixed solvent of dimethyl sulfoxide and dimethylformamide to prepare MAPbCl3The perovskite precursor solution is placed on a magnetic stirrer and stirred overnight at the temperature of 15-30 ℃;
weighing MABr and PbBr2Adding powder into dimethylformamide solvent to obtain MAPbBr3Placing the perovskite precursor solution on a magnetic stirrer, stirring overnight, and stirring overnight at 60 ℃;
s2. basic MAPbCl3Growing of single crystal:
the MAPbCl is subjected to3Filtering perovskite precursor solution into a clean bottle by adopting a polytetrafluoroethylene filter, subpackaging into 1ml of small bottles, placing on a 25 ℃ hot plate, raising and maintaining the temperature of the hot plate for the first time, raising and maintaining the temperature of the hot plate for the second time, and preparing MAPbCl3And (3) single crystal.
S3. heterogeneous MAPbCl3-MAPbBr3Growing of single crystal:
sequentially cleaning two glass substrates in a detergent, deionized water, acetone and isopropanol by ultrasonic waves, and cleaning the glass substrates and MAPbCl3Placing the single crystal into a clean glass bottle, and placing glass substrates on the bottom and top of the single crystal respectively to limit heterogeneous MAPbCl3-MAPbBr3Single crystal growth in a specific direction was carried out by placing the glass vial on a hot plate at 60 ℃ and MAPbBr3Pouring the precursor solution into a glass bottle, sealing, slowly heating and maintaining to obtain heterogeneous MAPbCl3-MAPbBr3Treating the single crystal with MACl isopropanol solution to obtain heterogeneous MAPbCl treated with MACl isopropanol solution3-MAPbBr3Single crystal;
s4, preparing the perovskite single crystal photoelectric detector:
heterogeneous MAPbCl treated with mask in MACl isopropanol solution3-MAPbBr3Evaporating Au electrode with size of 1mm × 1mm in single crystal center and depositing in heterogeneous MAPbCl3-MAPbBr3Au electrodes are simultaneously evaporated on the periphery of the single crystal, the thickness of the electrodes is 50nm,and manufacturing the perovskite single crystal photoelectric detector.
Preferably, in step S1, the MACl and PbCl are combined2The molar ratio of the powder is 1: 1, the volume ratio of dimethyl sulfoxide to dimethylformamide in the mixed solvent of dimethyl sulfoxide and dimethylformamide is 1: 1, the volume of the mixed solvent of dimethyl sulfoxide and dimethylformamide is 5 ml; the MAPbCl3The concentration of the perovskite precursor solution was 1M.
Preferably, in step S1, the MABr and PbBr are combined2The molar ratio of the powder is 1: 1, the volume of the dimethylformamide solvent is 5 ml; the MAPbBr3The concentration of the perovskite precursor solution was 1M.
Preferably, in step S2, the pore size of the teflon filter is 0.2 μm.
Preferably, in step S2, the temperature of the hot plate is raised for the first time and maintained at 45 ℃ for 5 hours.
Preferably, in step S2, the temperature of the hot plate is raised for the second time and maintained at 60 ℃ for 6 hours.
Preferably, in step S2, the MAPbCl3The size of the single crystal is 3-5 mm.
Preferably, in step S3, the temperature is slowly raised and maintained to 70 ℃ for 1 hour.
Preferably, in step S3, the MACl isopropanol solution treatment includes the following steps: spin coating 0.5mg/ml of MACl isopropanol solution at 4000rpm onto heterogeneous MAPbCl3-MAPbBr3Single crystal surface for 20 seconds, then heterogeneous MAPbCl3-MAPbBr3The single crystal was annealed at 60 ℃ for 10 minutes.
On the other hand, the invention also protects the perovskite single crystal photoelectric detector prepared by the preparation method.
The invention has the beneficial effects that:
(1) the preparation method of the perovskite single crystal photoelectric detector provided by the invention is simple to operate, has stable technology, has no strict requirements on preparation environment, is easy to obtain raw materials, has excellent effect, can keep stable work in air environment, and solves the technical problem that the detector can work without connecting an external voltage.
(2) The perovskite single crystal photoelectric detector provided by the invention has the characteristic of self-driving, has higher spectral responsivity and environmental stability, and can be used for detecting long-term optical signals.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1(a) shows MAPbCl in a heterojunction single crystal prepared by the example3Partially scanning electron microscope images;
FIG. 1(b) shows MAPbBr in the heterojunction single crystal prepared in example3Partially scanning electron microscope images;
FIG. 2 is an X-ray diffraction pattern of the heterojunction single crystal obtained in example;
FIG. 3 is MAPbCl3Single crystal, MAPbBr3Absorption profiles of three perovskite single crystals of the single crystal and the heterojunction single crystal prepared in example;
FIG. 4 is MAPbCl3Single crystal, MAPbBr3Spectral responsivity curves of the single crystal and the heterojunction single crystal prepared in the example and I-t curve graphs under monochromatic illumination of 400nm and 570 nm;
FIG. 5 is a graph of the stability test of the heterojunction single crystal prepared in the present example in an air environment;
fig. 6 shows an imaging system and a gray-scale value curve using the heterojunction single-crystal photodetector manufactured in this embodiment as a sensing pixel;
fig. 7 is a schematic structural view of the heterojunction single-crystal photodetector manufactured in this embodiment.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
The embodiment provides a preparation method of a perovskite single crystal photoelectric detector, which comprises the following steps:
s1, preparation of a perovskite precursor solution:
a. weighing a mixture with a molar ratio of 1: 1 MACl and PbCl2And mixing the powder and the mixture, adding the mixture into a mixture with a volume ratio of 1: 1, 5ml of dimethyl sulfoxide and dimethylformamide mixed solvent are mixed together, and MAPbCl with the concentration of 1M is prepared3The perovskite precursor solution was placed on a magnetic stirrer and stirred at room temperature overnight.
b. Weighing a mixture with a molar ratio of 1: 1 MABr and PbBr2Powder, both mixed and added to 5ml dimethylformamide solvent, formulated to a concentration of 1M MAPbBr3The perovskite precursor solution was stirred overnight at 60 ° on a magnetic stirrer.
S2. basic MAPbCl3Growing of single crystal: the MAPbCl is subjected to3The precursor solution was filtered through a 0.2 μm pore size Polytetrafluoroethylene (PTFE) filter into a clean bottle. To grow MAPbCl3Single crystal, the filtered precursor solutions were dispensed into vials (1 ml each), they were placed on a 25 ℃ hot plate, the temperature of the hot plate was raised to 45 ℃ and held for 5 hours, and heating was continued to raise the temperature of the hot plate to 60 ℃ and held for 6 hours. MAPbCl3 single crystals with a size of 3-5mm were then obtained.
S3. heterogeneous MAPbCl3-MAPbBr3Growth of single crystal (heterojunction single crystal): the heterojunction single crystal grows by a space confinement method and an inverse temperature crystallization method. And sequentially cleaning the two glass substrates in a detergent, deionized water, acetone and isopropanol by ultrasonic waves. Cleaning the glass substrate and MAPbCl3Placing the single crystal into a clean glass bottle, and placing glass substrates on the bottom and top of the single crystal to limitThe growth of the heterojunction single crystal towards a specific direction is made. The vials were placed on a hot plate at 60 ℃. Then, MAPbBr was added3The precursor solution was poured into a glass bottle and sealed. The temperature was slowly raised to 70 ℃ and held for 1 hour. Then, a heterojunction single crystal is obtained. The obtained heterojunction single crystal was treated with MACl isopropanol solution. A MACl isopropanol solution (0.5mg/ml) was spin-coated on the surface of the heterojunction single crystal (4000rpm, 20s), and then the heterojunction single crystal was annealed at 60 ℃ for 10 minutes.
S4, preparing the perovskite single crystal photoelectric detector: and evaporating an Au electrode with the size of 1mm multiplied by 1mm on the center of the heterogeneous single crystal by using a mask, and simultaneously evaporating Au electrodes on the periphery of the heterogeneous single crystal, wherein the thickness of the electrodes is 50nm, thus obtaining the perovskite single crystal photoelectric detector.
Test examples
Examination of heterogeneous MAPbCl made in example3-MAPbBr3Surface morphology and Properties of Single crystals (heterojunction Single crystals)
1. Analysis by scanning Electron microscope
Scanning electron microscope analysis is carried out on the heterojunction single crystal, and as shown in figure 1, the defect-free surface and high growth quality of the heterojunction single crystal prepared by the embodiment can be obviously observed in figure 1.
XRD analysis
XRD analysis is carried out on the heterojunction single crystal, as shown in figure 2, the diffraction peak reflected by the curve in figure 2 is highly matched with each crystal face, and no redundant diffraction peak appears after the heterojunction single crystal is grown, which indicates that the perovskite single crystal prepared by the embodiment has high synthesis quality.
3. Spectral absorption analysis
Spectral absorption analysis was performed on the heterojunction single crystal, and as shown in FIG. 3, it can be seen from the absorption curve in FIG. 3 that the light absorption positions of the heterojunction single crystal produced in the example correspond to MAPbCl respectively3Single crystal and MAPbBr3The position of light absorption of the single crystal indicates the successful synthesis of two single crystals together by the method provided in the examples.
4. Spectral responsivity analysis
From the test curve of FIG. 4(a), the spectral response range at 0V is 250nm to 570 nm. The two cut-off wavelengths are located at ≈ 430nm and ≈ 570nm, respectively. The spectral responsivity above 570nm drops sharply, a result which is consistent with the absorption spectrum. The two peak responsivities are 26.8mA/W at 400nm and 0.21mA/W at 570nm, respectively.
Figure 4(b) shows the spectral responsivity curves of three single crystal devices under a bias of 1V. From the curves, it can be seen that the signal strength is measured by the MAPBCl curve3Lateral growth of MAPbBr around single crystal3Single crystal, enhanced response in the ultraviolet region. With MAPbCl3Compared with a single crystal device, the overall responsivity of the heterojunction single crystal device in an ultraviolet region is improved by nearly 470%. Due to the introduction of MAPbBr3The single crystal and heterojunction single crystal device still has spectral response in the range of 440-570 nm, but the responsivity is lower than MAPbBr3A single crystal device. This is because MAPbBr in heterojunction single crystal devices3The single crystal portion provides a carrier concentration less than pure MAPbBr3The carrier concentration provided by the single crystal device.
The I-t curves of the three single crystal devices under light irradiation with wavelengths of 400nm and 570nm under a bias of 1V are shown in FIGS. 4(c) and 4 (d). When 400nm monochromatic light is applied and removed, three photodetectors all produce periodically varying currents, indicating that the device has significant reproducibility and stability. Wherein, I of the heterojunction single-crystal device in FIG. 4(c)light/IdarkThe variation is greatest. MAPbCl when tested using 570nm monochromatic light3The single crystal device has no periodicity variation because 570nm is not within the applicable range of the device. MAPbBr in FIG. 4(d)3The photocurrent generated by the single crystal device is greater than that generated by the heterojunction device. This is due to pure MAPbBr3The concentration of photon-generated carriers generated by the single crystal is greater than MAPbBr of the heterojunction single crystal3The concentration of partially generated photogenerated carriers. This phenomenon is consistent with the responsivity spectrum of fig. 4 (b). In addition, the spectral response of the heterojunction single-crystal photodetector can be tested without any external power supply, proving the possibility of the invention.
5. Stability test of heterojunction single crystal in air environment
The spectral responsivity change condition of the heterojunction single crystal within 120 days is tested, and the curve in fig. 5 shows that the spectral responsivity hardly changes in an atmospheric environment with humidity of 40%, so that the heterojunction single crystal photoelectric detector prepared by the embodiment of the invention has high air stability and can be used for long-term optical signal detection.
6. Imaging capability of heterojunction single-crystal photoelectric detector under 0V
In order to test the imaging capability of the heterojunction single-crystal self-powered photodetector at 0V, an imaging system using the heterojunction single-crystal photodetector manufactured in the present embodiment as a sensing pixel was constructed, as shown in fig. 6(a) below.
An object (school badge of harbin university) with a hollowed pattern is manufactured on a steel plate by a laser cutting machine and is used as a target object of an imaging system. The object is mounted on a computer-controlled X-Y translation stage that is continuously movable in both horizontal and vertical directions. Using a 405nm laser (5mW) as a test light source, the photocurrent generated by the photodetector was extracted and recorded by a lock-in amplifier and a computer as the translation stage was moved, and recorded simultaneously with the position coordinates of the object. Then, an image is acquired by combining the current intensity and position coordinates, as shown in fig. 6 (b). From the image, it can be observed that the test image has a clear boundary, which is highly consistent with the shape of the target object. The gray values were extracted along the dotted line labeled in fig. 6(b) using MATLAB, as shown in fig. 6 (c). The gray scale value changes from high to low and corresponds to the image boundary. The heterojunction single-crystal photoelectric detector is adopted as a sensing pixel, and the imaging system has high fidelity. These results indicate that the heterojunction single-crystal photodetector provided by the present invention can meet the requirements of an imaging system without any external power supply.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.

Claims (10)

1. A preparation method of a perovskite single crystal photoelectric detector is characterized by comprising the following steps: the preparation method comprises the following steps:
s1, preparation of a perovskite precursor solution:
weighing MACl and PbCl2Adding the powder into a mixed solvent of dimethyl sulfoxide and dimethylformamide to prepare MAPbCl3The perovskite precursor solution is placed on a magnetic stirrer and stirred overnight at the temperature of 15-30 ℃;
weighing MABr and PbBr2Adding powder into dimethylformamide solvent to obtain MAPbBr3Placing the perovskite precursor solution on a magnetic stirrer, stirring overnight, and stirring overnight at 60 ℃;
s2. basic MAPbCl3Growing of single crystal:
the MAPbCl is subjected to3Filtering perovskite precursor solution into a clean bottle by adopting a polytetrafluoroethylene filter, subpackaging into 1ml of small bottles, placing on a 25 ℃ hot plate, raising and maintaining the temperature of the hot plate for the first time, raising and maintaining the temperature of the hot plate for the second time, and preparing MAPbCl3Single crystal;
s3. heterogeneous MAPbCl3-MAPbBr3Growing of single crystal:
sequentially cleaning two glass substrates in a detergent, deionized water, acetone and isopropanol by ultrasonic waves, and cleaning the glass substrates and MAPbCl3Placing the single crystal into a clean glass bottle, and placing glass substrates on the bottom and top of the single crystal respectively to limit heterogeneous MAPbCl3-MAPbBr3Single crystal growth in a specific direction was carried out by placing the glass vial on a hot plate at 60 ℃ and MAPbBr3Pouring the precursor solution into a glass bottle, sealing, slowly heating and maintaining to obtain heterogeneous MAPbCl3-MAPbBr3Treating the single crystal with MACl isopropanol solution to obtain heterogeneous MAPbCl treated with MACl isopropanol solution3-MAPbBr3Single crystal;
s4, preparing the perovskite single crystal photoelectric detector:
heterogeneous MAPbCl treated with mask in MACl isopropanol solution3-MAPbBr3Evaporating Au electrode with size of 1mm × 1mm in single crystal center and depositing in heterogeneous MAPbCl3-MAPbBr3And simultaneously evaporating Au electrodes around the single crystal, wherein the thickness of the electrodes is 50nm, and thus the perovskite single crystal photoelectric detector is prepared.
2. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S1, the MACl and PbCl are performed2The molar ratio of the powder is 1: 1, the volume ratio of dimethyl sulfoxide to dimethylformamide in the mixed solvent of dimethyl sulfoxide and dimethylformamide is 1: 1, the volume of the mixed solvent of dimethyl sulfoxide and dimethylformamide is 5 ml; the MAPbCl3The concentration of the perovskite precursor solution was 1M.
3. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S1, the MABr and PbBr are2The molar ratio of the powder is 1: 1, the volume of the dimethylformamide solvent is 5 ml; the MAPbBr3The concentration of the perovskite precursor solution was 1M.
4. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S2, the pore size of the ptfe filter is 0.2 μm.
5. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S2, the temperature of the hot plate is raised for the first time and maintained at 45 ℃ for 5 hours.
6. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S2, the temperature of the hot plate is raised for the second time and maintained at 60 ℃ for 6 hours.
7. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S2, the MAPbCl is set3The size of the single crystal is 3-5 mm.
8. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S3, the temperature is slowly raised and maintained at 70 ℃ for 1 hour.
9. The method for producing a perovskite single crystal photodetector as claimed in claim 1, wherein: in step S3, the treatment with MACl isopropanol solution includes the following steps: spin coating 0.5mg/ml of MACl isopropanol solution at 4000rpm onto heterogeneous MAPbCl3-MAPbBr3Single crystal surface for 20 seconds, then heterogeneous MAPbCl3-MAPbBr3The single crystal was annealed at 60 ℃ for 10 minutes.
10. A perovskite single crystal photodetector produced by the production method described in any one of claims 1 to 9.
CN202210085136.1A 2022-01-25 2022-01-25 Perovskite single crystal photoelectric detector and preparation method thereof Pending CN114530560A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115161760A (en) * 2022-07-12 2022-10-11 吉林大学 Double perovskite transverse heterojunction prepared by two-step nanoimprint method, preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115161760A (en) * 2022-07-12 2022-10-11 吉林大学 Double perovskite transverse heterojunction prepared by two-step nanoimprint method, preparation method and application thereof
CN115161760B (en) * 2022-07-12 2023-10-31 吉林大学 Double perovskite transverse heterojunction prepared by two-step nanoimprint method, preparation method and application thereof

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