CN110649162A - Wide-spectrum self-driven inorganic perovskite photoelectric detector and preparation method thereof - Google Patents

Wide-spectrum self-driven inorganic perovskite photoelectric detector and preparation method thereof Download PDF

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CN110649162A
CN110649162A CN201910910003.1A CN201910910003A CN110649162A CN 110649162 A CN110649162 A CN 110649162A CN 201910910003 A CN201910910003 A CN 201910910003A CN 110649162 A CN110649162 A CN 110649162A
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曹风人
李亮
田维
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Abstract

The invention relates to a wide-spectrum self-driven perovskite photoelectric detector and a preparation method thereof, wherein the wide-spectrum self-driven perovskite photoelectric detector comprises a conductive substrate, an electron transmission layer, a lead-based perovskite nano concave-convex structure, an organic conjugated polymer layer and an electrode layer which are sequentially arranged; the material of the organic conjugated polymer layer comprises PDPP3T and/or P3 HT. The preparation method comprises the following steps: forming an oxide layer on the surface of the conductive substrate; then spin-coating a precursor solution of the lead-based perovskite material on the surface of the oxide layer, and forming a lead-based perovskite nano concave-convex structure by adopting an imprinting technology; and sequentially forming an organic conjugated polymer layer and an electrode layer on the surface of the lead-based perovskite nano concave-convex structure, wherein the organic conjugated polymer layer is made of PDPP3T and/or P3 HT. The photoelectric detector of the invention has simple preparation method, self-driving property and proper energy band structure, is beneficial to improving the separation of electron hole pairs, has high light absorption and utilization rate, and effectively improves the performance of the photoelectric detector.

Description

Wide-spectrum self-driven inorganic perovskite photoelectric detector and preparation method thereof
Technical Field
The invention relates to the field of photoelectric detectors, in particular to a wide-spectrum self-driven perovskite photoelectric detector and a preparation method thereof.
Background
In recent centuries, with the rapid development of science and technology, the demand for energy has also increased rapidly. However, non-renewable traditional energy sources (coal, petroleum and natural gas) still occupy the leading position (> 85%) worldwide at present, and the proportion of the non-renewable traditional energy sources in China is more than 90%. Meanwhile, the coal energy which has the most serious environmental pollution in the energy structure of China is as high as 60%, and the number is far higher than 29% in the energy structure of the world. China is a country with large energy consumption, the environmental problem caused by the unreasonable energy structure is particularly serious, the potential damage to economy is huge, and meanwhile, the unavoidable influence can be brought to social life. In order to solve the problem, the existing energy structure must be changed, and sustainable green energy is developed. But changing the energy structure is not done all at once, which is a lengthy process. From the perspective of human safety, effective monitoring means must be provided to detect the harm, so as to solve the harm and guarantee the safety of human life.
Among various monitoring sensors, a photodetector that converts an optical signal into an electrical signal is of great importance. The human eye can directly observe the optical band about 400-760nm, but the whole optical band (10-10)6nm) is very small. The appearance and development of photoelectric detectors enable human beings to more comprehensively recognize light, so that the photoelectric detectors have a wide application basis in the fields of industrial and scientific research, such as environmental pollution detection, ozone layer cavity monitoring, security inspection, optical communication, medical diagnosis, flame detection, infrared night vision and the like. However, the balance between performance and cost still exists, and high performance is accompanied by high cost.
In recent years, the emerging lead-based perovskite material has attracted the extensive research interest of researchers in the materials for preparing the photoelectric detector. The absorption coefficient is high, and exciton combination is low; the energy band position of the material can be adjusted by adjusting the ion proportion in the material, so that the material is convenient to match with the energy bands of other semiconductor materials; the lead-based perovskite has long diffusion coefficient and high carrier mobility, and can effectively separate and transmit carriers; and good solution processability and low-temperature crystallinity are beneficial to the perovskite to adapt to different preparation modes. But the perovskite material has the problems of not wide response range, poor stability of hybrid perovskite and the like, and further development of the perovskite material is limited. Therefore, it is very important to fully utilize the advantages of the lead-based perovskite, improve the defects thereof, design a reasonable composite structure to reduce the cost and meet the new development trend (self-driving property, flexibility and multifunctionality).
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a wide-spectrum self-driven perovskite photoelectric detector and a preparation method thereof.
The invention provides a wide-spectrum self-driven perovskite photoelectric detector, which comprises a conductive substrate, an electron transmission layer, a lead-based perovskite nano concave-convex structure, an organic conjugated polymer layer and an electrode layer which are sequentially arranged; the organic conjugated polymer layer is made of polythiophene-pyrrolopyrrole dione (PDPP3T) and/or 3-hexyl-substituted polythiophene (P3 HT).
Furthermore, the conductive substrate is made of fluorine-doped tin oxide (FTO) conductive glass or Indium Tin Oxide (ITO).
Further, the material of the electron transport layer is metal oxide, preferably, the metal oxide is tin oxide (SnO)2) Titanium oxide (TiO)2) Or zinc oxide (ZnO). More preferably, the metal oxide is SnO2
Further, the thickness of the electron transport layer is 10nm to 100nm, preferably 50 to 70nm, and more preferably 60 nm.
Further, the lead-based perovskite nano concave-convex structure is a nanowire array structure and comprises a plurality of perovskite nanowires which are parallel to each other, the perovskite nanowires are perpendicular to the conductive substrate, the period of the perovskite nano concave-convex structure is 7500 (the area of a device is adjustable, the period number is variable according to the length), the grating constant is 100-300nm, the groove depth is 80-200nm, and the width is 100-200 nm. Compared with a common film structure, the nano concave-convex structure is beneficial to light convergence, improves the light utilization rate and further improves the performance of the photoelectric detector.
Furthermore, the lead-based perovskite nano concave-convex structure is made of CsPbBr3、MAPbI3And the like. Preferably, the lead-based perovskite nano concave-convex structure is made of CsPbBr3
Further, the organic conjugated polymer layer comprises a PDPP3T layer and a P3HT layer, the thickness of the PDPP3T layer is 80-150nm (preferably 80-100nm), and the thickness of the P3HT layer is 80-150nm (preferably 80-100 nm).
Further, the thickness of the electrode layer is 50-200 nm. Preferably 90-100 nm.
Preferably, the material of the electrode layer is silver.
Preferably, the wide-spectrum self-driven perovskite photoelectric detector comprises conductive glass and SnO which are sequentially arranged from bottom to top2Layer, CsPbBr3Nano-concave-convex structure, PDPP3T layer, P3HT layer and electrode layer.
Further, the spectral response range of the broad-spectrum self-driven perovskite photodetector is 350-950 nm.
On the other hand, the invention also provides a preparation method of the wide-spectrum self-driven perovskite photoelectric detector, which comprises the following steps:
(1) forming an electron transport layer on the surface of the conductive substrate;
(2) coating a precursor solution of the lead-based perovskite material on the surface of one side of the electron transport layer, which is far away from the conductive substrate, and forming a lead-based perovskite nano concave-convex structure by adopting an imprinting technology;
(3) and sequentially forming an organic conjugated polymer layer and an electrode layer on the surface of one side of the lead-based perovskite nano concave-convex structure, which is far away from the electron transmission layer, wherein the organic conjugated polymer layer is made of PDPP3T and/or P3HT, so that the wide-spectrum self-driven perovskite photoelectric detector is obtained.
Further, in the step (1), the material of the electron transport layer is a metal oxide. And coating the precursor solution of the electron transport layer on the surface of the conductive substrate by adopting a coating method.
Further, in the step (2), the concentration of the precursor solution of the lead-based perovskite material is 0.1-0.4 mol/L.
Preferably, the precursor solution of the lead-based perovskite material is CsPbBr3The preparation method of the precursor solution comprises the following steps:
adding cesium bromide and lead bromide into a DMSO solution, and stirring for more than 3h under a closed condition at the temperature of 60-70 ℃. The molar ratio of cesium bromide to lead bromide is 1:1, and the concentration is 0.1-0.4 mol/L. The container equipped with the solution is a sealable capped bottle.
Further, the precursor solution of the lead-based perovskite material must be a transparent yellow uniform solution, so that the purity of the prepared material is ensured, and the phenomenon of uneven deposition cannot occur.
Further, in the step (2), the lead-based perovskite nano concave-convex structure is a nanowire array.
Further, in the step (2), the imprinting time is 1-5min, and the imprinting temperature is 150-. Varying the imprinting time or temperature can alter the purity and imprinting morphology of the perovskite.
Further, in the step (2), an imprinting template with a nano concave-convex structure is adopted for imprinting, and the imprinting template is a commercial DVD-R, CD-R optical disk or PDMS.
Further, in the step (2), the pressure applied by the template is 0.4-1.0 MPa.
Further, in the step (3), a PDPP3T solution and a P3HT solution are sequentially coated on the surface of the lead-based perovskite nano concave-convex structure by a coating method, wherein the concentration of the PDPP3T solution is 0.1-7mg/mL, and the concentration of the P3HT solution is 0.1-25 mg/mL.
The solvent for the PDPP3T solution and the P3HT solution is benzene-based solvent such as chlorobenzene, toluene, or phenetole.
Furthermore, in the present invention, the coating method is preferably a spin coating method, and the spin coating speed is 2000-.
Further, an electrode layer was prepared by an evaporation method.
The invention provides a method for preparing a wide-spectrum self-driven perovskite photoelectric detector by using a composite inorganic perovskite and an organic conjugated polymer. The composition of the structure widens the spectral response range of the perovskite, enhances the generation, separation and transmission of current carriers, and provides self-driving property.
By the scheme, the invention at least has the following advantages:
the semiconductor photoelectric detector is obtained by compounding the lead-based perovskite nano concave-convex structure and the organic conjugated polymer, and separation and transmission of photon-generated carriers can be effectively promoted. Compared with a single perovskite photoelectric detector, the photoelectric detector has a wider spectral response range (the spectral response range is widened from 530nm to 950nm), and the responsivity and the response speed performance are improved; the nanometer concave-convex structure at the bottom is beneficial to light convergence, the utilization of light is improved, and the performance of the photoelectric detector is further improved; meanwhile, due to the existence of the heterojunction structure, the photoelectric detector has self-driving performance, namely, a working power supply is not required to be provided from the outside, so that the miniaturization and the simplification of the device are facilitated, and the application range of the device is widened. Therefore, the photoelectric detector prepared by the method has feasibility and broad prospect.
The method has the advantages of simple preparation process and sufficient raw materials. Is beneficial to the future industrialized production and has great potential application value.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a sectional SEM (scanning electron microscope) view of a photodetector prepared in example 1 of the present invention;
FIG. 2 is a graph showing responsivity and specific detectivity of the photodetector prepared in example 1 of the present invention under different optical bands;
FIG. 3 is a response speed curve of a photodetector manufactured in example 1 of the present invention in an optical band of 405 nm;
FIG. 4 is a stability curve of the photodetector prepared in example 1 of the present invention in 0V air.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The invention prepares the inorganic perovskite material compound machine conjugated polymer to obtain the wide-spectrum self-driven perovskite photoelectric detector. The method comprises the steps of firstly forming a tin oxide film on conductive glass through spin coating to serve as an electron transport layer, and removing residual solvent through a 60 ℃ drying process. And then forming the perovskite nanowire array on the tin oxide film by combining a spin coating method and an imprinting method. Finally, the organic conjugated polymer is used as a spectrum broadening material and a hole transmission material is covered on CsPbBr3And the nanowire arrays are arranged. In the present invention, the prepared photodetector can be directly used for detecting elements, and in the following embodiments, the photodetector prepared by the present invention is directly used as an element to test the detection performance.
Example 1
(1) The ITO conductive glass is ultrasonically cleaned for 20 minutes according to the sequence of acetone, alcohol and deionized water. Drying the cleaned conductive glass, performing ultraviolet ozone treatment for 20min, and measuring 0.05mL SnO by using a liquid transfer gun2The precursor solution is spin-coated on the conductive glass, the spin-coating speed is 5000r/min, the acceleration is 1000 r/s, and the spin-coating time is 30 s. Then placing the spin-coated sample on a heating table at 60 ℃ to heat for 30min, namely forming a layer of SnO on the surface of the conductive substrate2A film.
(2) 0.085g of cesium bromide and 0.147g of lead bromide are added into 1mL of DMSO, and the mixture is stirred at 70 ℃ for 3 hours to react to obtain a yellow, transparent and uniform perovskite precursor solution. And (3) measuring 0.05mL of perovskite precursor solution by using a liquid transfer gun, spin-coating the perovskite precursor solution on the sample prepared in the step (1), and immediately carrying out imprinting by using DVD-R as a template, wherein the imprinting temperature is 180 ℃, the imprinting time is 3 minutes, and the pressure is 0.6 MPa. Cooling to obtain cesium lead bromide (CsPbBr) after imprinting3) And (4) nanowire arrays.
(3) Respectively dissolving 5mg of PDPP3T and 15mg of P3HT in 1mL of chlorobenzene, stirring at 70 ℃ for 12 hours to obtain uniform solutions, measuring 0.05mL of the solutions by using a liquid transfer gun in sequence, spin-coating the solutions on the nanowire array sample prepared in the step (1), wherein the spin-coating speed is 2000 rpm, the acceleration is 1000 rpm, and finally, evaporating and coating silver to be used as a top electrode.
The photoelectric detector prepared by the steps comprises conductive glass and SnO which are sequentially arranged from bottom to top2Layer (about 60nm), CsPbBr3Nano-relief structures (period 7500, grating constant about 300nm, trench depth about 100nm, width about 250nm), a PDPP3T layer (about 100nm), a P3HT layer (about 100nm) and an electrode layer (about 90 nm). The cross-sectional topography of the final composite photodetector is shown in figure 1. From FIG. 1, it can be seen that the successful formation of nanowire arrays, without CsPbBr in-between the nanowires, is achieved3The residue of (1). In addition, the organic conjugated polymer can well cover the nanowire array and has good delamination. From the theoretical simulation results, under different light irradiation, the light is converged in different areas compared with the complete thin film sample due to the existence of the bottom nanowire array. Under the illumination of different wavelengths, different layers of materials are respectively used as main light absorption layers, so that the separation and transmission processes of carriers are influenced.
The device is used as a photoelectric detection element, and then the response performance of the device is tested under different wavelengths of light, and the result is shown in figure 2. As can be seen from the figure, under the wavelength light of 300-950nm, the responsivity of the photoelectric detector prepared by the method of the invention is still as high as 0.2A W without adding an external working voltage source-1The specific detectivity is 1013Jones. Furthermore, inThe response speed is 111/306 mus at the light wave band of 405nm (shown in figure 3). For practical applications, stability is also important, and as can be seen from fig. 4, in a test of high-power white light continuously over a long time, the photocurrent of the sample is only attenuated by 10% at 20 hours, while a fast response speed is still maintained, which indicates that the photodetector prepared by the method has good stability.
Example 2
A composite photodetector was prepared as in steps (1) to (3) of example 1, except that the mass of PDPP3T and P3HT in step (3) was reduced to 1mg and 5mg, respectively. The performance of the composite photodetector prepared was slightly lower than that of example 1.
Example 3
A composite photodetector was prepared as in steps (1) to (3) of example 1 except that the imprint temperature in step (2) was decreased to 160 ℃. The performance of the composite photodetector prepared was slightly lower than that of example 1.
Example 4
A composite photodetector was produced as in steps (1) to (3) of example 1 except that the conductive glass in step (1) was changed to FTO conductive glass. The performance of the composite photodetector prepared was close to that of example 1.
Example 5
A composite photodetector was prepared as in steps (1) - (3) of example 1, except that in step (3), only the PDPP3T solution was spin coated onto the nanowire array samples, and finally silver was evaporated as the top electrode.
Using the above device as a photodetector, the responsivity of the prepared photodetector is lower than that of the photodetector in example 1, and even lower than 1/4 in example 1 at the wavelength of light higher than 550nm at the wavelength of light of 300-950 nm.
Example 6
A composite photodetector was prepared as in steps (1) to (3) of example 1, except that, in step (3), 5mg of PDPP3T and 15mg of P3HT were mixed and dissolved in 1mL of chlorobenzene, the resulting mixed solution was spin-coated on the nanowire array sample, and finally silver was evaporated as a top electrode.
The prepared photoelectric detector has lower responsivity than that of the photoelectric detector in example 1 and less responsivity than 1/2 in example 1 under the wavelength of light higher than 550nm by using the device as a photoelectric detection element under the wavelength of light of 300-950 nm.
The method has the advantages of simple process, wide spectral response range of the photoelectric detector, high response speed and high responsiveness, and has huge potential application value. The photoelectric detector prepared by the method has self-driving property, and is convenient for miniaturization and portability; the proper energy band structure is beneficial to improving the separation of electron hole pairs; compared with the traditional film structure, the grating structure is beneficial to improving the absorption and utilization of light, and the performance of the photoelectric detector is effectively improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A wide-spectrum self-driven perovskite photodetector is characterized in that: the lead-based perovskite nano concave-convex structure comprises a conductive substrate, an electron transmission layer, a lead-based perovskite nano concave-convex structure, an organic conjugated polymer layer and an electrode layer which are sequentially arranged; the material of the organic conjugated polymer layer comprises PDPP3T and/or P3 HT.
2. The broad spectrum self-driven perovskite photodetector of claim 1, wherein: the lead-based perovskite nano concave-convex structure comprises a plurality of perovskite nano wires which are parallel to each other, the perovskite nano wires are perpendicular to the conductive substrate, the grating constant of the perovskite nano concave-convex structure is 100-300nm, the groove depth is 80-200nm, and the width is 100-200 nm.
3. The broad spectrum self-driven perovskite photodetector of claim 1, wherein: the organic conjugated polymer layer comprises a PDPP3T layer and a P3HT layer, the thickness of the PDPP3T layer is 80-150nm, and the thickness of the P3HT layer is 80-150 nm.
4. The broad spectrum self-driven perovskite photodetector of claim 1, wherein: the thickness of the electron transport layer is 10-100 nm.
5. The broad spectrum self-driven perovskite photodetector of claim 1, wherein: the electron transport layer is made of metal oxide.
6. The broad spectrum self-driven perovskite photodetector of claim 1, wherein: the thickness of the electrode layer is 50-200 nm.
7. A method of fabricating a broad spectrum self-driven perovskite photodetector as defined in any one of claims 1 to 6 comprising the steps of:
(1) forming an electron transport layer on the surface of the conductive substrate;
(2) coating a precursor solution of the lead-based perovskite material on the surface of one side of the electron transport layer, which is far away from the conductive substrate, and forming a lead-based perovskite nano concave-convex structure by adopting an imprinting technology;
(3) and sequentially forming an organic conjugated polymer layer and an electrode layer on the surface of one side of the lead-based perovskite nano concave-convex structure, which is far away from the electron transmission layer, wherein the organic conjugated polymer layer is made of PDPP3T and/or P3HT, so that the wide-spectrum self-driven perovskite photoelectric detector is obtained.
8. The method of claim 7, wherein: in the step (2), the concentration of the precursor solution of the lead-based perovskite material is 0.1-0.4 mol/L.
9. The method of claim 7, wherein: in the step (2), the imprinting time is 1-5min, and the imprinting temperature is 150-.
10. The method of claim 7, wherein: in the step (3), a PDPP3T solution and a P3HT solution are sequentially coated on the surface of the lead-based perovskite nano concave-convex structure by a coating method, wherein the concentration of the PDPP3T solution is 0.1-7mg/mL, and the concentration of the P3HT solution is 0.1-25 mg/mL.
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CN115148904B (en) * 2022-05-23 2024-03-19 苏州大学 Transparent and stable all-inorganic metal halogen perovskite photoelectric detector and preparation method and application thereof

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