CN110676342B - Perovskite material-based X-ray detector and preparation method thereof - Google Patents
Perovskite material-based X-ray detector and preparation method thereof Download PDFInfo
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L31/08—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
- H01L31/10—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 characterised by at least one potential-jump barrier or surface barrier, e.g. phototransistors
- H01L31/115—Devices sensitive to very short wavelength, e.g. X-rays, gamma-rays or corpuscular radiation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention relates to an X-ray detector based on perovskite materials and a preparation method thereof, wherein the method comprises the following steps: step 1, preparing a mixture of a raw material and a solvent according to a molar ratio of 3:2 weighing AI and BI3Dissolving raw materials in an organic solvent to obtain a mixed precursor liquid; wherein AI is CsI, CH3NH3I or RbI; BI (BI)3Is BiI3Or Sbi3(ii) a Step 2, sealing the mixed precursor liquid, heating to 60-100 ℃, keeping for 2-48 hours to ensure that the mixed precursor liquid is fully dissolved and balanced, and taking supernate to obtain a fully saturated solution of the precursor; step 3, placing the fully saturated solution of the precursor at an ambient temperature lower than the heating termination temperature in the step 2, gradually heating at a speed of less than 5 ℃/day until crystals are precipitated, and stopping heating after the temperature is continuously increased by at most 10 ℃ to obtain A3B2I9A perovskite single crystal; step 4, taking out and drying the single crystal; and 5, evaporating an interdigital metal electrode on the surface of the single crystal.
Description
Technical Field
The invention relates to the field of semiconductor X-ray detectors, in particular to an X-ray detector based on perovskite materials and a preparation method thereof.
Background
The semiconductor radiation detector has been widely applied to industries such as national defense and military, medical health, public safety, high-end industry, scientific research and the like by virtue of the advantages of high energy resolution, high detection efficiency, large stopping power and the like. The semiconductor detector for detecting radioactive rays directly converts absorbed ray energy into electron-hole pairs, and the electron-hole pairs drift under the action of an external electric field to output signals. In practical application, different semiconductors are selected as light absorption layer materials of the detector according to different applications. Currently in the medical field, digital medical imaging has become an important part of current medical diagnostic treatment. In recent years, X-ray Flat Panel Detectors (FPDs) have received much attention and research due to their excellent imaging performance. The X-ray flat panel detector is divided into a direct type and an indirect type, and compared with the direct type flat panel detector, the direct type flat panel detector has better spatial resolution and simpler system device. Direct X-ray flat panel detectors using α -Se, Si and CdZnTe as light absorbing layers have been commercially used. However, these materials still have problems such as complicated preparation process, high price, low sensitivity due to small atomic number of the material, and insufficient detection dose. Therefore, the development of new semiconductor materials with higher sensitivity and lower detection limit for X-rays is very urgent and necessary.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an X-ray detector based on perovskite material and a preparation method thereof, and the X-ray detector based on perovskite material A3B2I9The perovskite type single crystal has the advantages of simple preparation method, no toxicity, no pollution and low cost, and the obtained semiconductor X-ray detector has high detection sensitivity, low detection limit and high stability.
The invention is realized by the following technical scheme:
x-ray detector based on perovskite material, comprising A as light-absorbing layer3B2I9A perovskite-type material and an electrode provided on one surface thereof.
Preferably, A is3B2I9In the perovskite-type material, A is CH3NH3 +，Cs+Or Rb+(ii) a B is Bi3+Or Sb3+。
Preferably, A is3B2I9The perovskite material is A3B2I9A type of single crystal material.
Preferably, the electrodes are metal interdigital electrodes.
Further, the electrode is a gold electrode or a copper electrode.
The preparation method of the X-ray detector based on the perovskite material comprises the following steps:
step 4, taking out and drying the single crystal;
and 5, evaporating an interdigital metal electrode on the surface of the single crystal to obtain the semiconductor X-ray detector.
Preferably, the concentration of the mixed precursor liquid is 0.2 to 1.5 mol/L.
Preferably, the organic solvent is at least one of γ -butyrolactone, N-dimethylformamide, dimethyl sulfoxide and N-methyl-2-pyrrolidone.
Preferably, in step 3, the fully saturated solution of the precursor is placed at an ambient temperature 2-5 ℃ lower than the termination temperature of heating in step 2.
Preferably, in step 3, the temperature is maintained or increased by a further maximum of 10 ℃ until crystals precipitate, and then the temperature is stopped.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adopts A3B2I9Perovskite single crystal is taken as light absorption layer to prepare X-ray detector, and is taken as A of light absorption layer3B2I9The perovskite single crystal has large atomic number, high absorption coefficient to rays, high carrier mobility and long service life, and is beneficial to realizing higher ray sensitivity; the relatively large resistivity is beneficial to realizing lower detection limit; the heat stability and the humidity stability are good; the interdigital electrode arranged on one side surface is matched, so that the X-ray detection interdigital electrode has a simple structure, a short preparation process flow and low cost, direct and rapid derivation of electrons and holes is realized, and extremely high X-ray detectability is realizedCan be used.
The invention can obtain the fully saturated solution of the precursor and simultaneously fully remove impurities and precipitated mixed crystals in the solution by sealing, heating and maintaining the mixed precursor solution. Meanwhile, the initial temperature of crystal growth is lower than the holding temperature of sealing and heating, so that the continuous and stable rate can be kept when the single crystal is separated out, and the forming quality of the crystal is ensured. After the crystal is precipitated, the temperature is continuously raised at a certain rate or kept for a period of time, so as to fully utilize solute in the precursor solution and grow and obtain crystals with larger size.
Drawings
Fig. 1 is a schematic structural diagram of an X-ray detector based on perovskite material according to an embodiment of the present invention. In the figure, first and second interdigital electrodes 1 and 2 and a light absorption layer 3 are shown.
Fig. 2 is a graph of attenuation efficiency versus thickness for 40KeV energy radiation for the different materials described in the examples of the present invention.
FIG. 3 is an I-t plot of 40KeV energy lines measured by the X-ray detector in an example of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The X-ray detector based on the perovskite material comprises A as an absorption layer of the device3B2I9A perovskite-type single crystal and an interdigital electrode arranged on the surface of the absorption layer. The method is that the growth A is controlled in the solution3B2I9The perovskite single crystal is used as a ray absorption layer, and then an interdigital electrode is evaporated on the surface of the perovskite single crystal to collect electrons and holes, so that the device assembly is directly completed in one step. The semiconductor X-ray detector has the advantages of simple method and process, high response sensitivity, low detection limit, environmental friendliness, long service life and the like, and has wide application prospect.
Specifically, the perovskite material-based X-ray detector comprises: a. the3B2I9Perovskite type single crystal and interdigital electrode prepared on the surface of the single crystal. It is composed ofIn (A)3B2I9The perovskite single crystal is used as the light absorption layer material of the X-ray detector, A is CH3NH3 +，Cs+，Rb+(ii) a B is Bi3+，Sb3+. The interdigital electrode is a metal electrode, gold (Au) or copper (Cu).
The invention relates to a preparation method of an X-ray detector based on a perovskite material, which specifically comprises the following steps:
step 4, taking out and drying the single crystal;
and 5, evaporating an interdigital metal electrode on the surface of the single crystal to obtain the semiconductor X-ray detector. The metal interdigital electrode is an Au electrode or a Cu electrode.
A obtained in the preferred embodiment3B2I9Perovskite Single Crystal X-ray Detector, as shown in FIG. 1, A3B2I9The perovskite single crystal is used as a light absorption layer 3, and a pair of first and second interdigital electrodes 1, 2 are oppositely arranged above the light absorption layer. A. the3B2I9The perovskite is a defective perovskite material, and the existing perovskite materialThe material is easy to nucleate in large quantity by a solution growth method, crystal growth is mainly controlled by nucleation, so that polycrystal or twin crystal is formed, and large-size bulk single crystal with high quality and low defect is difficult to obtain. Therefore, the invention controls the nucleation quantity by reducing the nucleation sites, so that the dominant crystal nucleus preferentially grows, and good single crystal crystals are obtained. In the steps 2 and 3, the mixed precursor liquid is put into a crystallizing dish for sealing, heated to 60-100 ℃, and kept for 2-48 hours, so that a large number of active sites which are easy to nucleate are eliminated, and meanwhile, the solution is ensured to reach the optimal saturated state, so that the solution is fully dissolved and balanced; taking supernatant in a crystallizing dish, placing the supernatant in a 60-100 ℃ oven, gradually heating at a speed of less than 5 ℃/day, and after a large number of nucleation sites are eliminated, controlling crystal precipitation by temperature regulation, thereby growing to obtain high-quality A3B2I9A perovskite single crystal.
Compared with the traditional up-down structure, the planar structure X-ray detector prepared by the arranged interdigital electrodes has the advantages of simple preparation process, low cost and easy integration. Most importantly, the X-ray detector with the planar structure prepared by the interdigital electrode has lower detection limit and higher response speed, which is beneficial to reducing the dosage of the X-ray detector and shortening the radiation time, thereby greatly reducing the radiation injury to patients in medical use.
As shown in FIG. 2, A of the present invention3B2I9Perovskite single crystal as absorption layer, and other Si, C, Cs2AgBiBr6，MAPbI3Compared with the prior art, the method has the obvious advantage that the attenuation efficiency of rays is higher under the same thickness. Compared with the material prepared by the X-ray detector used for commercial use at present, the X-ray detector based on the perovskite material has larger average relative atomic number because of containing heavy atoms of Cs, Bi and I. (the larger the atomic number, the stronger the attenuation of X-rays), so A3B2I9Perovskite type is a very good X-ray absorbing material; in addition, experiments have demonstrated that this material is comparable to previous perovskites (MAPbI)3，MAPbBr3，Cs2AgBiBr6) Has better properties, such as low dark current, small ion migration and excellent stability. The low dark current of the semiconductor photoelectric material has the advantages that the intrinsic carrier concentration of the material is low, the noise current generated as a device is low, and particularly for X-rays, the detection limit can be effectively reduced; since the X-ray detector generally needs to work under a large electric field, ion migration is easily caused, and the ion migration may cause structural damage of the material, resulting in rapid decomposition. In addition, the ion migration can affect the working stability of the device, shorten the service life, and also cause the problems of unstable detection signals, poor imaging quality, reduced resolution ratio and the like. Since perovskite is a soft lattice material, the ion migration problem is very common, so that the problem of ion migration can be effectively solved by growing the perovskite crystal, and the stability of the perovskite crystal is ensured.
As shown in FIG. 3, the I-t curve of the X-ray detector based on perovskite material under the irradiation of 40KeV ray under the condition of applying an electric field of 1.5V/mum is shown in FIG. 3, when the ray is switched and circulated, the X-ray detector has high on-off current ratio and good detection performance.
Example 1
step 4, taking out the crystal and drying;
and 5, evaporating an Au electrode on the surface of the crystal.
Example 2
step 4, taking out the crystal and drying;
and 5, evaporating an Au electrode on the surface of the crystal.
Example 3
step 4, taking out the crystal and drying;
and 5, evaporating a Cu electrode on the surface of the crystal.
Example 4
step 4, taking out the crystal and drying;
and 5, evaporating a Cu electrode on the surface of the crystal.
Example 5
step 4, taking out the crystal and drying;
and 5, evaporating a Cu electrode on the surface of the crystal.
Example 6
step 4, taking out the crystal and drying;
and 5, evaporating a Cu electrode on the surface of the crystal.
Example 7
step 4, taking out the crystal and drying;
and 5, evaporating an Au electrode on the surface of the crystal.
Example 8
step 4, taking out the crystal and drying;
and 5, evaporating an Au electrode on the surface of the crystal.
Example 9
step 4, taking out the crystal and drying;
and 5, evaporating an Au electrode on the surface of the crystal.
Example 10
step 4, taking out the crystal and drying;
and 5, evaporating an Au electrode on the surface of the crystal.
Claims (5)
1. The preparation method of the X-ray detector based on the perovskite material is characterized by comprising the following steps:
step 1, preparing a mixture of a raw material and a solvent according to a molar ratio of 3:2, weighing AI and BI3 raw materials, and dissolving the raw materials in an organic solvent to obtain a mixed precursor liquid; wherein AI is CsI or RbI; BI3 is BiI3 or SbI 3;
step 2, sealing the mixed precursor liquid, heating to 60-100 ℃, keeping for 2-48 hours to ensure that the mixed precursor liquid is fully dissolved and balanced, and taking supernate to obtain a fully saturated solution of the precursor;
step 3, placing the fully saturated solution of the precursor at an ambient temperature which is 2-5 ℃ lower than the heating termination temperature in the step 2, gradually heating at a speed of less than 5 ℃/day until crystals are precipitated, and keeping the temperature or stopping heating after the temperature is continuously increased by at most 10 ℃ to obtain the A3B2I9 perovskite single crystal;
step 4, taking out and drying the single crystal;
and 5, evaporating an interdigital metal electrode on the surface of the single crystal to obtain the X-ray detector based on the perovskite material.
2. The method for preparing an X-ray detector based on perovskite material according to claim 1, wherein the concentration of the mixed precursor liquid is 0.2-1.5 mol/L.
3. The method for preparing an X-ray detector based on perovskite material as claimed in claim 1, wherein the organic solvent is at least one of γ -butyrolactone, N-dimethylformamide, dimethyl sulfoxide and N-methyl-2-pyrrolidone.
4. An X-ray detector based on perovskite material, characterized in that it is made by the manufacturing method according to any one of the preceding claims 1 to 3.
5. The perovskite material-based X-ray detector of claim 4, wherein the electrode is a gold electrode or a copper electrode.
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| CN112071989B (en) * | 2020-09-14 | 2022-05-31 | 吉林大学 | Perovskite single crystal-based X-ray detector and preparation method thereof |
| CN113046830B (en) * | 2021-02-25 | 2023-07-18 | 上海大学 | Mixed solvent-based all-inorganic perovskite Cs 3 Sb 2 Cl 9 Single crystal growth method of (2) |
| CN113299837B (en) * | 2021-03-31 | 2022-10-21 | 西北大学 | Two-dimensional perovskite single crystal and preparation method of ion implantation-based detector thereof |
| CN113897681B (en) * | 2021-09-18 | 2022-11-01 | 湖北工业大学 | Preparation method of non-lead perovskite single crystal with (110) orientation |
| CN113889548B (en) * | 2021-10-18 | 2024-04-09 | 苏州亿现电子科技有限公司 | High-sensitivity detection structure based on perovskite avalanche transistor and preparation method |
| CN115196675A (en) * | 2022-08-23 | 2022-10-18 | 上海应用技术大学 | Preparation method of lead-free perovskite crystal material |
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