CN113026102A - Inorganic perovskite material, photoelectric detector and preparation method thereof - Google Patents
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Abstract
The invention relates to the field of inorganic perovskite materials, in particular to an inorganic perovskite material, a photoelectric detector and a preparation method thereof. The invention adopts the hot isostatic pressing method to prepare the all-inorganic perovskite polycrystalline bulk material from the inorganic perovskite powder, and uses the excimer laser to carry out surface modification on the inorganic perovskite polycrystalline bulk material. The hot isostatic pressing preparation method is simple, the material utilization rate is higher, the method is more universal, devices in any shapes can be prepared according to requirements, and the post-processing is more convenient; the laser modification can simply and quickly reduce the surface defects of the inorganic perovskite polycrystalline block material, and the time consumption is short, and no new chemical reagent needs to be introduced. And then, evaporating an Au interdigital electrode on the surface of the inorganic perovskite material to obtain the photoelectric detector. The method is suitable for research and commercial production of photoelectric detectors based on inorganic perovskite materials, and has good application prospect.
Description
Technical Field
The invention discloses the field of inorganic perovskite-based materials, and particularly relates to an inorganic perovskite material, a photoelectric detector and a preparation method of the inorganic perovskite material.
Background
Perovskite materials have many excellent properties, such as high optical absorption coefficient, high carrier mobility, long carrier diffusion length, and the like. The properties can well meet the requirements of high-efficiency photoelectric devices, so that the perovskite material has wide application prospects in the fields of photoelectric detection, ray detection, solar cells and the like. For example, over a decade of development, the photoelectric conversion efficiency of polycrystalline perovskite thin film solar cells increased from 3.8% in 2009 to 25.5% in 2021, exceeding the efficiency record of polycrystalline silicon solar cells (23.3%), approaching that of monocrystalline silicon solar cells (26.1%) [ Prog photo voltaic Res appl, 2021,29, 3-15%]. However, the organic Cation (CH) in the organic-inorganic hybrid perovskite material3NH3 +、CH(NH2)2 +) The material is extremely sensitive to environmental humidity, so that the environmental stability and the thermal stability of the material are poor, and the further development of the organic-inorganic hybrid perovskite material is limited. Inorganic cations (Cs) for all-inorganic perovskite materials, as compared to organic-inorganic hybrid perovskites+) Substituted organic Cation (CH)3NH3 +、CH(NH2)2 +) Exhibits better environmental stability and thermal stability, causeThe wide focus of researchers. For example, in 2017, a university of Nanjing Physician, the team of professor H.Zeng, cooperated with a university of Shanghai applied technology, the team of professor J.xu, prepared CsPbBr by Bridgman method3The single crystal and the photoelectric detector prepared on the basis of the single crystal show that the responsivity of the detector to light with the wavelength of 535nm reaches 2A/W under the bias voltage of 5V, which is much higher than that of the commercial silicon-based detector (the structure is shown in the specification: (the structure is shown in the specification))<0.2A/W). In addition, under the bias of 5V, the responsivity of the infrared band is 1.4mA/W, which is comparable to that of a commercial Si and GaAs two-photon detector [ adv]。
Surface defects are one of the important factors affecting the performance of optoelectronic devices. For example, when the inorganic perovskite photodetector works, a photogenerated carrier can be collected by an Au electrode only through an interface between a perovskite material and the Au electrode, and the surface defect of the inorganic perovskite material can form a charge trap to capture a part of the carrier, so that the performance of the device is influenced; meanwhile, the surface defects can also increase the dark current of the photoelectric detector and reduce the on-off ratio of an important performance index of the photoelectric detector. There are also studies on the reduction of surface defects in inorganic perovskite materials, e.g., professor j. huang, 2020 to obtain CsPbBr with regular shape and less surface defects3Single crystal blocks of CsPbBr prepared by reverse temperature crystallization process3After polishing the single crystal with sand paper, spin-coating the surface thereof (C)8H17NH3)2SO4And CsPbBr3Reaction to produce PbSO4A passivation layer, effectively passivates CsPbBr3Surface of material [ J.Mater.chem.C., 2020,8,11360-11368 ]]. Although some progress has been made in reducing surface defects of inorganic perovskites and improving device performance, the process is complicated and requires additional chemical reagents. If a method for controlling the surface defects of the inorganic perovskite material, which is simple and rapid and does not need additional chemical reagents, can be developed, the research and the practicability of the all-inorganic perovskite-based device can be promoted.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defect that CsPbBr with regular shape and less surface defects is obtained in the prior art3The defects that the process of the single crystal block is complicated and additional chemical reagents are needed are overcome, and the inorganic perovskite material, the preparation method thereof and the photoelectric detector prepared from the inorganic perovskite material are provided.
In order to solve the technical problem of the invention, the technical scheme is that the preparation method of the inorganic perovskite material is characterized in that the structural formula of the inorganic perovskite is ABX3Wherein A is Cs, B is one or the compound of two or more of Pb, Bi and Sn, and X is one or the compound of two or more of Cl, Br and I, the method comprises the following steps:
s1, preparing inorganic perovskite powder;
s2, preparing the inorganic perovskite powder material obtained in the step S1 into an inorganic perovskite polycrystalline bulk material by a hot isostatic pressing method;
and S3, carrying out surface modification on the inorganic perovskite polycrystalline bulk material by using an excimer laser.
The preparation method of the inorganic perovskite material is further improved as follows:
preferably, the inorganic perovskite powder material in the step S1 is prepared from AX and BX2The inorganic perovskite single crystal is prepared by a crystallization method and then is ground into powder.
Preferably, the crystallization method is one of an anti-solvent diffusion method, an inverse temperature crystallization method and a solvent evaporation crystallization method.
Preferably, the inorganic perovskite powder material in the step S1 is prepared from AX and BX2Mixing and grinding to fully react to obtain the catalyst.
Preferably, in the hot isostatic pressing method described in step S2, the temperature of the hot isostatic pressing machine is 150-600 ℃, and the pressure is 1-200 MPa.
Preferably, the excimer laser in step S2 is ArF excimer laser with a wavelength of 193nm, KrF excimer laser with a wavelength of 248nm, XeCl excimer laser with a wavelength of 308nm, or XeF excimer laser with a wavelength of 351 nm.
Preferably, the excimer laser generates the UV pulse laser energy density of 50 μ J/cm in step S22-50mJ/cm2Frequency of operationThe rate is 1-200Hz, and the pulse number of laser irradiation to the inorganic perovskite material is 1-4000.
In order to solve another technical problem of the invention, the technical scheme is that the inorganic perovskite material is prepared by any one of the preparation methods.
In order to solve another technical problem of the invention, the technical scheme is that the photoelectric detector is made of the inorganic perovskite material, and the photoelectric detector is obtained by evaporating Au interdigital electrodes on the surface of the inorganic perovskite material. .
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a method for preparing an all-inorganic perovskite polycrystalline block material by adopting a hot isostatic pressing method. Compared with the perovskite single crystal prepared by the traditional solution method or melt method, the hot isostatic pressing preparation method is simple, the material utilization rate is higher, the method is more universal, devices in any shapes can be prepared according to requirements, and the later-stage processing is more convenient.
2. The invention provides a method for reducing surface defects of an inorganic perovskite polycrystalline block material by utilizing excimer laser surface modification. Laser modification is less time consuming than conventional surface modification and modification techniques and does not require the introduction of new chemical reagents. Different from the conventional laser modification for surface modification of materials through thermal action, the quasi-laser used in the invention has short wavelength and high photon energy, breaks chemical bonds in molecules and generates photochemical action; in addition, the method provided by the invention is simple and easy to control, the energy density, the frequency, the irradiation time, the pulse number and the like of the laser can be accurately controlled, and the surface modification effect has excellent repeatability.
Drawings
FIG. 1 shows CsPbBr before and after laser modification in examples 1 and 23Cross-sectional SEM images of the polycrystalline blocks.
FIG. 2 shows the CsPbBr prepared in example 13The photoelectric detector has a photoresponse performance curve under the irradiation light source wavelength of 530nm and different optical power densities; wherein a is an I-V curve of the device in a dark state and at different optical power densities; b diagram of the on-off ratio of the device as a function of voltageCurve line.
FIG. 3 is a diagram of preparation of laser modified CsPbBr in example 23The photoelectric detector has a photoresponse performance curve under the irradiation light source wavelength of 530nm and different optical power densities; wherein a is an I-V curve of the device in a dark state and at different optical power densities; graph b is a plot of switching ratio of the device as a function of voltage.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative effort based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
(1) CsPbBr preparation by anti-solvent diffusion method3Single crystal: 3.3g of PbBr were weighed2And 1.4g CsBr in 15ml DMSO and stirred for more than one hour. Filtering the precursor solution with organic syringe filter to obtain clear solution, and filtering the clear solution with CH3OH titration until an orange yellow precipitate precipitates, filtration again to give a clear solution, which is transferred to a CH-filled container3In the environment of OH steam, the ambient temperature is kept at 20 ℃, and CsPbBr is obtained after one-week growth3And (3) single crystal.
(2)CsPbBr3Preparing powder: 1.3g of CsPbBr were weighed3The single crystals were ground into a powder in an agate mortar.
(3) Hot isostatic pressing CsPbBr3Preparing a polycrystalline block material: reacting CsPbBr3Placing the powder in a hot isostatic pressing machine, setting the pressure at 20MPa, the temperature at 200 ℃ and the heating time at 8h to prepare CsPbBr3Polycrystalline block material;
(4) ordinary CsPbBr3Preparing a photoelectric detector: in CsPbBr3Evaporating Au interdigital electrodes on the polycrystalline block material to obtain common CsPbBr3A photodetector.
Example 2
(1)CsPbBr3Laser surface modification of polycrystalline blocks: using a KrF excimer laser of 248nm to convert the energy of the laser into energyThe mass density was set to 10mJ/cm2The laser operating frequency was set to 10Hz, and CsPbBr prepared in step (3) of example 1 was used3Irradiating the polycrystalline block material with the number of irradiation pulses of 30 to obtain laser modified CsPbBr3Polycrystalline block material;
(2)CsPbBr3preparing a photoelectric detector: CsPbBr after laser surface modification3Evaporating Au interdigital electrode on the polycrystalline block material to obtain CsPbBr3A photodetector.
CsPbBr before and after laser modification in examples 1 and 23The results of scanning SEM images of the cross sections of the polycrystalline bulk materials are shown in FIGS. 1a and 1b, respectively, and it can be seen from FIG. 1 that CsPbBr was present before and after laser modification3The surface of the polycrystalline block is free of small particles CsPbBr3The crystal grain appearance is sharper, the crystal boundary is clearer, and the surface quality of the material is obviously improved.
The photo-response performance curves of the electric detectors prepared in the example 1 and the example 2 under the conditions of the wavelength of the test irradiation light source being 530nm and different optical power densities are shown in the following figures 2 and 3 respectively: wherein FIGS. 2a and 3a are I-V curves of the device in the dark state and at different optical power densities; fig. 2b and 3b are graphs of the switching ratio of the device as a function of voltage. The curve shows that the CsPbBr is modified by laser3The dark current of the polycrystalline block material is reduced by 4 orders of magnitude compared with that before the polycrystalline block material is not modified, and the dark current is reduced by 4.14mW/cm2Under the light intensity and the bias of 1V, the on-off ratio is improved from less than 10 to more than 1000, and the photoelectric detection performance is obviously improved.
It should be understood by those skilled in the art that the foregoing is only illustrative of several embodiments of the invention, and not of all embodiments. It should be noted that many variations and modifications are possible to those skilled in the art, and all variations and modifications that do not depart from the gist of the invention are intended to be within the scope of the invention as defined in the appended claims.
Claims (9)
1. A preparation method of an inorganic perovskite material, wherein the structural formula of the inorganic perovskite is ABX3Wherein A is Cs, B is one or the composition of two or more of Pb, Bi and Sn, and X is Cl, Br and IThe method is characterized by comprising the following steps:
s1, preparing inorganic perovskite powder;
s2, preparing the inorganic perovskite powder material obtained in the step S1 into an inorganic perovskite polycrystalline bulk material by a hot isostatic pressing method;
and S3, carrying out surface modification on the inorganic perovskite polycrystalline bulk material by using an excimer laser.
2. The method according to claim 1, wherein the inorganic perovskite powder of step S1 is prepared from AX and BX2The inorganic perovskite single crystal is prepared by a crystallization method and then is ground into powder.
3. The method of claim 2, wherein the crystallization process is one of an anti-solvent diffusion process, an inverse temperature crystallization process, and a solvent evaporation crystallization process.
4. The method according to claim 1, wherein the inorganic perovskite powder of step S1 is prepared from AX and BX2Mixing and grinding to fully react to obtain the catalyst.
5. The method of claim 1, wherein the hot isostatic pressing is performed at a temperature of 150 ℃ and a pressure of 1-200MPa in step S2.
6. The method according to claim 1, wherein the excimer laser in step S2 is ArF excimer laser with a wavelength of 193nm, KrF excimer laser with a wavelength of 248nm, XeCl excimer laser with a wavelength of 308nm, or XeF excimer laser with a wavelength of 351 nm.
7. The method of claim 1The preparation method of the inorganic perovskite material is characterized in that the energy density of ultraviolet pulse laser generated by the excimer laser in the step S2 is 50 mu J/cm2-50 mJ/cm2The working frequency is 1-200Hz, and the pulse number for laser irradiation of the inorganic perovskite material is 1-4000.
8. An inorganic perovskite material produced by the production method according to any one of claims 1 to 7.
9. A photodetector made of the inorganic perovskite material as claimed in claim 8, wherein the photodetector is obtained by vapor deposition of Au interdigital electrodes on the surface of the inorganic perovskite material.
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Cited By (2)
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| CN116847665A (en) * | 2023-09-01 | 2023-10-03 | 济南大学 | Silicon-based epitaxial perovskite heterogeneous PN junction photoelectric detector and preparation method thereof |
| WO2024098487A1 (en) * | 2022-11-08 | 2024-05-16 | 深圳先进技术研究院 | All-inorganic perovskite photosensitive layer, and preparation method therefor and use thereof |
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| CN107919409A (en) * | 2017-09-20 | 2018-04-17 | 湖北大学 | One kind is based on CsPbBr3Visible ray photodetector of full-inorganic perovskite nano wire and preparation method thereof |
| CN108682746A (en) * | 2018-04-25 | 2018-10-19 | 中国科学院合肥物质科学研究院 | A kind of surface is modified organic inorganic hybridization perovskite material and method of modifying and application |
| CN110484963A (en) * | 2019-08-13 | 2019-11-22 | 山东大学 | A kind of method that pressure-driven ion diffusion growth prepares inorganic perovskite monocrystal thin films |
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| WO2024098487A1 (en) * | 2022-11-08 | 2024-05-16 | 深圳先进技术研究院 | All-inorganic perovskite photosensitive layer, and preparation method therefor and use thereof |
| CN116847665A (en) * | 2023-09-01 | 2023-10-03 | 济南大学 | Silicon-based epitaxial perovskite heterogeneous PN junction photoelectric detector and preparation method thereof |
| CN116847665B (en) * | 2023-09-01 | 2023-12-19 | 济南大学 | Silicon-based epitaxial perovskite heterogeneous PN junction photoelectric detector and preparation method thereof |
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