CN113130769A - Two-dimensional layered perovskite single crystal, wide-spectrum photoelectric detector and preparation method thereof - Google Patents

Two-dimensional layered perovskite single crystal, wide-spectrum photoelectric detector and preparation method thereof Download PDF

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CN113130769A
CN113130769A CN202110386089.XA CN202110386089A CN113130769A CN 113130769 A CN113130769 A CN 113130769A CN 202110386089 A CN202110386089 A CN 202110386089A CN 113130769 A CN113130769 A CN 113130769A
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perovskite single
perovskite
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CN113130769B (en
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李格非
吕俊鹏
张勇
倪振华
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Southeast University
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Abstract

The invention discloses a novel two-dimensional layered perovskite single crystal and a preparation method of a photoelectric detector thereof, which comprises the following steps: (1) preparing perovskite precursor solution, dissolving 2-bromoethylamine hydrobromide and lead oxide in hydrobromic acid hypophosphorous acid mixed solution to prepare precursor solution; (2) stirring at high temperature until the solution is transparent, and slowly cooling to obtain perovskite single crystal; (3) thermally evaporating an electrode; (4) mechanically stripping to obtain two-dimensional perovskite single crystal; (5) the obtained two-dimensional perovskite single crystal is transferred onto an electrode. The novel perovskite single crystal of the present invention has high crystal quality and a large crystal volume. The photoelectric detector based on the perovskite has a wide spectral response range from ultraviolet 325nm to near infrared 800nm, and has huge application potential in the fields of visible light communication and light sensing.

Description

Two-dimensional layered perovskite single crystal, wide-spectrum photoelectric detector and preparation method thereof
Technical Field
The invention belongs to the field of photoelectric conversion materials and devices, and particularly relates to a two-dimensional layered perovskite single crystal, a wide-spectrum photoelectric detector and a preparation method thereof.
Background
Organic-inorganic hybrid lead-halogen perovskites are receiving wide attention due to their adjustable band gap, high quantum yield, low production cost, and the like. However, the conventional three-dimensional perovskite has limited further commercial development due to problems such as poor stability. For this reason, the formation of a layered perovskite structure by introducing a cation containing a hydrophobic group is considered to be an effective means for improvement. However, the photoelectric properties of the layered perovskite are generally poor because the introduced long-chain cations are insulating. Furthermore, the current research on layered perovskites is mainly based on Butylamine (BA) and Phenethylamine (PEA) cations, and relatively few studies on other novel layered perovskite materials are performed, which is obviously disadvantageous for finding suitable substitutes which have both good stability and inherit the excellent performance of three-dimensional perovskites. The novel layered perovskite is explored to enrich the perovskite system material types, so that the performance of the perovskite photoelectric device is expected to be further improved, and the basic photophysical properties of the perovskite are more favorably researched.
The photoelectric detector has wide application in biomedical imaging, optical sensing, environmental monitoring and the like. Obtaining highly sensitive wide-spectrum photodetectors covering the ultraviolet-visible band is the hot direction of research therein. The low-dimensional perovskite is expected to be a candidate material for preparing a high-sensitivity photoelectric detector due to the advantages of high carrier mobility, high absorbance and the like. However, due to the limitation of the forbidden band width of the low-dimensional perovskite material, how to realize a wide detection range covering the full visible spectrum still faces huge challenges.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a novel two-dimensional layered perovskite single crystal and a preparation method thereof, and the invention also aims to provide a wide-spectrum photoelectric detector capable of breaking through band gap limitation and a preparation method thereof, wherein the wide-spectrum photoelectric detector has a wide detection range covering ultraviolet (325nm) -near infrared (800 nm).
The technical scheme is as follows: a preparation method of a two-dimensional layered perovskite single crystal comprises the following steps:
(a1) preparing a perovskite precursor solution: dissolving 2-bromoethylamine hydrobromide and lead oxide in a hydrobromic acid hypophosphorous acid mixed solution to prepare a precursor solution;
(a2) stirring the precursor solution at the temperature of 80-120 ℃ until the precursor solution is colorless, and slowly cooling to obtain BEA2PbBr4PerovskiteAnd (3) single crystal. The single crystal itself is a layered, i.e. two-dimensional material, and the crystals are stacked together in many layers as the growth is completed.
Further, the molar ratio of 2-bromoethylamine hydrobromide to lead oxide in step (a1) is 2: 1 to 5: 1, preferably 4: 1; the volume ratio of hydrobromic acid to hypophosphorous acid in step (a1) is 7: 1 to 11: 1, preferably 10: 1.
Further, the concentration of lead oxide in the precursor solution in the step (a1) is 0.8 to 1.4M, preferably 1.1M.
Further, the slow cooling rate in the step (a2) is 0.5 ℃. h-1-5℃·h-1。
BEA prepared by the preparation method2PbBr4A perovskite single crystal.
A method for preparing a wide-spectrum photodetector comprises the following steps:
(b) preparing an electrode;
(c) mechanically stripping the BEA according to claim 62PbBr4A perovskite single crystal;
(d) the BEA obtained after stripping in (b2)2PbBr4The perovskite single crystal is transferred to an electrode.
Further, the thickness of the electrode in the step (b) is 20-80nm, and the material is one or more of gold, silver and aluminum.
Further, the width of the electrode channel in the step (b) is 5um-200 μm.
Further, the post mechanical stripping BEA described in step (c)2PbBr4The thickness of the perovskite single crystal is 20-600 nm.
A wide-spectrum photoelectric detector prepared by the preparation method.
Has the advantages that: novel BEA of the invention2PbBr4The perovskite single crystal has good crystal quality and large crystal size, the obtained photoelectric detector breaks through the limitation of forbidden bandwidth, obtains a wide detection range covering a visible light wave band, and has higher response rate.
Drawings
FIG. 1 is a schematic diagram of a device structure in the present invention;
FIG. 2 is a layered BEA of example 12PbBr4XRD patterns of perovskites;
FIG. 3 is a layered BEA of example 22PbBr4XRD patterns of perovskites;
FIG. 4 is a current-voltage curve for different illuminations for the broad spectrum photodetector of example 1;
FIG. 5 is a graph of the photoresponse of the broad spectrum photodetector of example 1 under 5V bias, 760nm laser illumination;
FIG. 6 is a graph of responsivity at different wavelengths normalized in example 1.
FIG. 7 is a graph of the responsivity of example 1 and example 3 at different wavelengths.
Detailed Description
For a further understanding of the present invention, reference will now be made in detail to the embodiments illustrated in the drawings.
Example 1
A preparation method of a two-dimensional layered perovskite single crystal and a wide-spectrum photoelectric detector thereof comprises the following steps:
(1) preparing a perovskite precursor solution: 1065.4mg of BEA & HBr and 290.2mg of PbO (4: 1) were weighed out using a ten-thousandth precision balance, and these drugs were dissolved together in 1.1ml of a mixed solvent of hydrobromic acid and hypophosphorous acid (the volume ratio of hydrobromic acid/hypophosphorous acid was 10/1);
(2) preparing novel layered perovskite single crystal: stirring the precursor solution in the step (1) at room temperature for 0.5 hour, and then continuously stirring at 120 ℃ for 2 hours; the precursor solution was quickly transferred to an oven at 1 ℃ h-1Cooling to room temperature;
(3) taking out the obtained layered perovskite single crystal, and drying in a vacuum drying oven for 12 hours;
(4) fixing a TEM grid on a silicon wafer by using PMMA, moving a sample into a vacuum evaporation chamber, and vacuumizing to 4 x 104Pa; under vacuum degree lower than 4 x 10-4Evaporating a metal electrode under Pa, and controlling the evaporation rate to be 0.1-0.2 angstrom/s; final thickness about 50 nm; and taking down the carrier net after evaporation.
(5) Mechanically stripping the two-dimensional perovskite single crystal obtained in the step (3) on PDMS by using an adhesive tape, wherein the thickness of the two-dimensional perovskite single crystal is 20 nm; and (4) transferring the mechanically stripped single crystal to the inter-electrode channel obtained in the step (4) by using a transfer table to obtain the wide-spectrum photoelectric detector.
(6) The devices were tested using an X-ray diffractometer, a 325nm laser, a 532nm laser, a 680-800nm continuous wavelength laser and a digital source meter.
Example 2
The difference from example 1 is that in step (1), the precursor solution is prepared: 225.379mg of BEA & HBr and 290.2mg of PbO (1: 1) were weighed out using a ten-thousandth precision balance, and these drugs were dissolved together in 1.1ml of a mixed solvent of hydrobromic acid and hypophosphorous acid (the volume ratio of hydrobromic acid/hypophosphorous acid was 10/1); the crystals prepared in this example had an XRD pattern (FIG. 3) in which a strong peak appeared at a higher diffraction order, indicating that the synthesized crystals were of poor quality, and in which quasi-two-dimensional BEA was present2BEAn- 1PbnBr3n+1(n-2, 3, 4.) the ratio of BEA-HBr to PbO will affect the crystal quality.
Example 3
The difference from the example 1 is that in the step (5), the two-dimensional perovskite single crystal obtained in the step (3) is mechanically peeled off on PDMS by using an adhesive tape, and the thickness of the two-dimensional perovskite single crystal is 600 nm; and (4) transferring the mechanically stripped single crystal to the inter-electrode channel obtained in the step (4) by using a transfer table to obtain the wide-spectrum photoelectric detector.
FIG. 1 is a schematic view of a device structure of the present invention comprising a substrate, a two-dimensional perovskite BEA2PbBr4Single crystal light absorbing layer, metal electrode.
FIG. 2 is an XRD pattern of the layered perovskite prepared in example 1 of the present invention; as shown in FIG. 2, the layered perovskite single crystal grown according to the present invention shows characteristic peaks belonging to the (00l) crystal plane of the layered perovskite.
FIG. 3 is an XRD pattern of the layered perovskite prepared in example 2 of the present invention;
FIG. 4 is a current-voltage curve for different illuminations of a broad spectrum photodetector; as shown in FIG. 4, the wide spectrum photodetector of the present invention has a reference number 10-15Ultra low dark current of AFlow, which indicates that the detector has a very high sensitivity.
FIG. 5 is a graph of the optical response of a broad spectrum photodetector under 5V bias, 760nm laser illumination; as shown in fig. 5, this shows that the wide-spectrum photodetector of the present invention has stable optical response characteristics and breaks through the limitation of the forbidden bandwidth.
FIG. 6 is a normalized responsivity curve at different wavelengths; as shown in fig. 6, the photodetector of the present invention has a wide detection range from ultraviolet (325nm) to near infrared (800nm), indicating that the photodetector is expected to function in the direction of optical communication and the like where high-sensitivity broad-spectrum detection is required.
FIG. 7 is a graph of responsivity versus wavelength for different thickness sample photodetectors; as shown in FIG. 7, the photodetectors with different thicknesses in the present invention have different responsivities and responsivity trend with wavelength, because the transmission depths of the different wavelengths are different according to the beer-Lambert absorption law, which indicates that we can adjust and control the response range of the detector by changing the thickness of the sample.

Claims (10)

1. A preparation method of a two-dimensional layered perovskite single crystal is characterized by comprising the following steps:
(a1) preparing a perovskite precursor solution: dissolving 2-bromoethylamine hydrobromide and lead oxide in a hydrobromic acid hypophosphorous acid mixed solution to prepare a precursor solution;
(a2) stirring the precursor solution at the temperature of 80-120 ℃ until the precursor solution is colorless, and slowly cooling to obtain BEA2PbBr4A perovskite single crystal.
2. The process of claim 1, wherein the molar ratio of 2-bromoethylamine hydrobromide to lead oxide in step (a1) is 2: 1 to 5: 1, and the volume ratio of hydrobromic acid to hypophosphorous acid in step (a1) is 7: 1 to 11: 1.
3. The method according to claim 1, wherein the concentration of lead oxide in the precursor solution in the step (a1) is 0.8 to 1.4M.
4. The method of claim 1, wherein the slow cooling rate in step (a2) is 0.5 ℃. h-1-5℃·h-1。
5. BEA prepared according to any one of claims 1 to 42PbBr4A perovskite single crystal.
6. A method for preparing a wide-spectrum photoelectric detector is characterized by comprising the following steps:
(b) preparing an electrode;
(c) mechanically stripping the BEA according to claim 52PbBr4A perovskite single crystal;
(d) the BEA obtained after stripping in (c) is treated2PbBr4The perovskite single crystal is transferred to an electrode.
7. The method according to claim 6, wherein the thickness of the electrode in step (b) is 20-80nm, and the material is one or more of gold, silver and aluminum.
8. The method of claim 6, wherein the width of the electrode channel in step (b) is 5um-200 μm.
9. The method of claim 6, wherein the mechanical stripping in step (c) results in a BEA2PbBr4The thickness of the perovskite single crystal is 20-600 nm.
10. A broad spectrum photodetector prepared according to any one of claims 6 to 9.
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CN114561708A (en) * 2022-03-01 2022-05-31 云南大学 Quasi-two-dimensional perovskite single crystal and preparation method thereof, perovskite photoelectric detector and preparation method thereof
CN114864745A (en) * 2022-05-10 2022-08-05 中国科学院半导体研究所 Preparation method of photoelectric detector
CN117080846A (en) * 2023-10-17 2023-11-17 长春理工大学 Novel two-dimensional perovskite coating transverse self-oscillation suppression mid-infrared laser

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CN114864745A (en) * 2022-05-10 2022-08-05 中国科学院半导体研究所 Preparation method of photoelectric detector
CN117080846A (en) * 2023-10-17 2023-11-17 长春理工大学 Novel two-dimensional perovskite coating transverse self-oscillation suppression mid-infrared laser

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