CN113026102B - Inorganic perovskite material, photoelectric detector and preparation method thereof - Google Patents
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/02—Production of homogeneous polycrystalline material with defined structure directly from the solid state
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
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- H01L31/08—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof in which radiation controls flow of current through the device, e.g. photoresistors
- H01L31/09—Devices sensitive to infrared, visible or ultraviolet radiation
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 coefficients, high carrier mobility, long carrier diffusion lengths, and the like. These properties are well satisfied withThe perovskite material has wide application prospect in the fields of photoelectric detection, ray detection, solar cells and the like due to the requirement of an effective photoelectric device. For example, over the course of ten years, 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 photovot Res appl.,2021,29, 3-15%]. However, the organic Cation (CH) in the organic-inorganic hybrid perovskite material 3 NH 3 + 、CH(NH 2 ) 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) 3 NH 3 + 、CH(NH 2 ) 2 + ) Shows better environmental stability and thermal stability, and attracts extensive attention 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 method 3 The 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 voltage 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 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 to reduce surface defects of inorganic perovskite materialsPrecisely, for example, in 2020, the professor group of J.Huang to obtain CsPbBr with regular shape and less surface defects 3 Single crystal blocks of CsPbBr prepared by reverse temperature crystallization process 3 After polishing the single crystal with sand paper, spin-coating the surface thereof (C) 8 H 17 NH 3 ) 2 SO 4 And CsPbBr 3 Reaction to produce PbSO 4 A passivation layer, effectively passivates CsPbBr 3 Surface of material [ J.Mater.chem.C,2020,8,11360-11368]. Although such methods have made some progress in reducing surface defects of inorganic perovskites and improving device performance, the process is cumbersome and requires additional chemical reagents. If a simple, fast, and no additional chemical reagent-based method for controlling surface defects of inorganic perovskite materials could be developed, it would be helpful to advance the research and practical application of all-inorganic perovskite-based devices.
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 art 3 The defects that the process of a monocrystalline block is more 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 ABX 3 Wherein 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 block material by a hot isostatic pressing method;
and S3, carrying out surface modification on the inorganic perovskite polycrystalline block by using an excimer laser.
The preparation method of the inorganic perovskite material is further improved as follows:
preferably, the inorganic perovskite powder material of the step S1 is prepared fromAX、BX 2 The 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 BX 2 Mixing and grinding to fully react to obtain the catalyst.
Preferably, in the hot isostatic pressing method used in step S2, the hot isostatic press is at a temperature of 150 to 600 ℃ and a pressure of 1 to 200MPa.
Preferably, the excimer laser in step S2 is ArF excimer laser with wavelength of 193nm, krF excimer laser with wavelength of 248nm, xeCl excimer laser with wavelength of 308nm, or XeF excimer laser with wavelength of 351 nm.
Preferably, the energy density of the ultraviolet pulse laser generated by the excimer laser in the step S2 is 50 muJ/cm 2 -50mJ/cm 2 The working frequency is 1-200Hz, and the pulse number for laser irradiation of 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 present invention, a technical solution is adopted in which the photodetector is made of the above inorganic perovskite material, and the photodetector 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 2 3 Cross-sectional SEM images of the polycrystalline blocks.
FIG. 2 shows the CsPbBr prepared in example 1 3 The photo-response performance curve of the photoelectric detector 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.
FIG. 3 is a diagram of preparation of laser modified CsPbBr in example 2 3 The photo-response performance curve of the photoelectric detector 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; and b is a graph of the 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 method 3 Single crystal: 3.3g of PbBr were weighed 2 And 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 CH 3 OH titration until precipitationThe orange precipitate was filtered again to give a clear solution which was transferred to a CH-filled container 3 In the environment of OH steam, the ambient temperature is kept at 20 ℃, and CsPbBr is obtained after one-week growth 3 And (3) single crystal.
(2)CsPbBr 3 Preparing powder: 1.3g of CsPbBr were weighed 3 The single crystals were ground in an agate mortar to a powder.
(3) Hot isostatic pressing CsPbBr 3 Preparing a polycrystalline block material: mixing CsPbBr 3 Placing 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 CsPbBr 3 Polycrystalline block material;
(4) Ordinary CsPbBr 3 Preparing a photoelectric detector: in CsPbBr 3 Evaporating Au interdigital electrode on the polycrystalline block material to obtain the common CsPbBr 3 A photodetector.
Example 2
(1)CsPbBr 3 Laser surface modification of polycrystalline blocks: using a 248nm KrF excimer laser, the energy density of the laser was set to 10mJ/cm 2 The laser operating frequency was set to 10Hz, and CsPbBr prepared in step (3) of example 1 was used 3 Irradiating the polycrystalline block material with the number of irradiation pulses being 30 to obtain the laser modified CsPbBr 3 Polycrystalline block material;
(2)CsPbBr 3 preparing a photoelectric detector: csPbBr after laser surface modification 3 Evaporating Au interdigital electrode on the polycrystalline block material to obtain CsPbBr 3 A photodetector.
CsPbBr before and after laser modification in examples 1 and 2 3 The 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 modification 3 The surface of the polycrystalline block is free of small particles CsPbBr 3 The 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 530nm of the test irradiation light source and different optical power densities are shown in the following figures 2 and 3 respectively: wherein FIGS. 2a and 3a show the dark state and different optical power densitiesThe I-V curve of the piece; 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 laser 3 The dark current of the polycrystalline block is reduced by 4 orders of magnitude compared with that before the polycrystalline block is modified, and is 4.14mW/cm 2 Under the light intensity of (2) and the bias of 1V, the on-off ratio is improved to more than 1000 from less than 10, 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 (5)
1. A preparation method of an inorganic perovskite material, wherein the structural formula of the inorganic perovskite is ABX 3 Wherein A is Cs, B is Pb, X is one or the combination of two or more of Cl, br and I, and the 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 block material by a hot isostatic pressing method;
s3, carrying out surface modification on the inorganic perovskite polycrystalline block by using an excimer laser;
the excimer laser is an ArF excimer laser with the wavelength of 193nm, a KrF excimer laser with the wavelength of 248nm, an XeCl excimer laser with the wavelength of 308nm or a XeF excimer laser with the wavelength of 351 nm; the energy density of the ultraviolet pulse laser generated by the excimer laser is 50 mu J/cm 2 -50 mJ/cm 2 The working frequency is 1-200Hz, and the pulse number for laser irradiation of the inorganic perovskite material is 1-4000.
2. The method according to claim 1, wherein the inorganic perovskite powder of step S1 is selected from the group consisting of AX and BX 2 Preparing inorganic perovskite single crystal by crystallization method, and grinding the inorganic perovskite single crystal into powderPulverizing to obtain the final product.
3. The method according to claim 2, wherein the crystallization method is one of an anti-solvent diffusion method, an inverse temperature crystallization method, and a solvent evaporation crystallization method.
4. The method according to claim 1, wherein the inorganic perovskite powder of step S1 is selected from the group consisting of AX and BX 2 Mixing and grinding to fully react to obtain the catalyst.
5. The process of claim 1, wherein the hot isostatic pressing is performed at a temperature of 150-600 ℃ and a pressure of 1-200MPa in step S2.
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| CN107919409B (en) * | 2017-09-20 | 2019-11-12 | 湖北大学 | One kind being based on CsPbBr3The visible light photodetector and preparation method thereof of full-inorganic perovskite nano wire |
| 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 |
| CN110484963B (en) * | 2019-08-13 | 2021-06-01 | 山东大学 | Method for preparing inorganic perovskite single crystal film by pressure-driven ion diffusion growth |
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