CN114361349A - Perovskite single crystal X-ray detector with small ion migration and manufacturing method - Google Patents

Perovskite single crystal X-ray detector with small ion migration and manufacturing method Download PDF

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CN114361349A
CN114361349A CN202111361430.2A CN202111361430A CN114361349A CN 114361349 A CN114361349 A CN 114361349A CN 202111361430 A CN202111361430 A CN 202111361430A CN 114361349 A CN114361349 A CN 114361349A
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single crystal
perovskite
perovskite single
mapbbr
ray detector
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顾豪爽
李晨曦
王钊
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Hubei University
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Abstract

The invention designs a perovskite single crystal X-ray detector with small ion migration and a manufacturing method thereof, the perovskite single crystal in the X-ray detector is prepared by a method of space limitation and inverse temperature crystallization and has MAPbBr of centimeter level3A perovskite single crystal comprising: preparing precursor solution of perovskite, preparing limited space and preparing MAPbBr3Perovskite single crystal and sputtering method on MAPbBr3Preparing electrodes on the perovskite single crystal and the like. The preparation of centimeter-scale MAPbBr3The perovskite single crystal handicraft is easy to be compatible and integrated with MEMS, the defect density is reduced, the fluorescence life is prolonged, the ion migration is inhibited by a method of regulating the molar ratio of the precursor solution, the process is simple, and the large-scale industrial production is easy to realize.

Description

Perovskite single crystal X-ray detector with small ion migration and manufacturing method
Technical Field
The invention relates to a perovskite single crystal X-ray detector with small ion migration and a manufacturing method thereof, belonging to the technical field of organic semiconductor materials and X-ray detectors.
Background
The X-ray not only has the general characteristic of light, but also has an important characteristic, namely penetrability, according to the characteristic, the X-ray is widely applied, not only can be used for carrying out perspective examination on the physical condition of a patient in the medical field, but also can be used in the fields of radiation therapy, industrial flaw detection, safety detection, aerospace navigation, material analysis of scientific research and the like, however, as the X-ray is widely applied in various industries, an operator is more or less directly contacted with the X-ray, practice proves that the radiation quantity of the weakly contacted X-ray exceeds a certain dosage, great harm can be generated to the human body, and even cell canceration can be caused seriously. Therefore, there is a need to research and develop a highly sensitive X-ray detector to facilitate the underlying labor protection.
Commercial X-ray detectors mainly employ two X-ray detection techniques: one is indirect detection, which uses a scintillator to indirectly convert X-rays into visible light, the scintillator mainly comprises PbWO4、Bi4Ge3O12、CsI:Tl、YAlO3Ce; another approach is direct detection; among the X-ray detectors that currently dominate the market, indirect detection with a scintillator as a material is most used. The direct detection adopts an absorption material to directly convert X-rays into electric signals, and the absorption material mainly comprises CdTe, CdZnTe and HgI2、PbI2The existing material for absorbing X-rays has low carrier mobility life product mu tau value and low charge collection efficiency due to low absorptivity of hard X-rays, and has the defects of absorptionThe material manufacturing process is complex and the cost is high. In the indirect detection, because the generated visible light is scattered in the process of converting X-ray high-energy photons into visible light by the scintillator, the spatial resolution and the quantum efficiency of the indirect X-ray detector are limited to a certain extent, for example, the technical scheme disclosed in the invention patent of 'a perovskite crystal/quantum dot composite scintillator and the preparation method and application thereof' (201811569753.9) has the problem that the visible light is scattered after the X-ray is converted into the visible light. Based on this, research and development of a sensitive and reliable X-ray detector based on direct detection are very important for the safety application of X-rays.
Research shows that the perovskite material has excellent performance in photoelectric detection, high carrier mobility and life product, large resistance, and very high atomic number (attenuation coefficient of X-ray is related to the material (alpha is in proportion to Z)4/E3) Z is the atomic number of a substance) and low cost, and the like, and becomes an ideal material for replacing the current material for preparing the X-ray detector.
In recent years, researchers have targeted MAPbI3Perovskite Single Crystal, MAPbBr3Perovskite Single Crystal and Cs2AgBiBr6The excellent performance of perovskite single crystal and other materials, a series of rapid and sensitive X-ray detectors based on a direct detection mode are designed. However, most of the absorbing materials in these detectors have the problems of unstable operation, low use repetition rate, low accuracy and the like caused by ion migration.
The technical schemes disclosed by the invention patents of ' halogenated perovskite single crystal, a preparation method and application thereof in the preparation of an X-ray detector ' (202010649024.5) ' an X-ray detector with energy resolution and a detection method thereof ' (201711381053.2) ' a perovskite single crystal X-ray detector and a preparation method thereof ' (201910066171.7) ' are based on MAPbBr3 perovskite single crystal materials for preparing the X-ray detector, but the technical schemes have the problem of ion migration, and in the processes of long-time work and repeated use for many times, the performance of the device can be gradually reduced and finally fails due to the problem of ion migration; the invention patent "a preparation method of a Cs2AgBiBr6 double perovskite crystal for X-ray detection" (201910693206. X) uses a Cs2AgBiBr6 double perovskite crystal to work under high voltage, and the same exists: the problems of ion migration, short service life of devices, poor stability and the like are easy to occur.
The invention patent 'an X-ray detector based on perovskite single crystal and a preparation method thereof' (202010959059.9) discloses a technical scheme which uses FAPBR 3 perovskite single crystal for preparation, and has the following defects: the FAPBBr3 perovskite single crystal material is easy to deliquesce, and the detection precision can be ensured only by using a dry environment.
Disclosure of Invention
The invention aims to solve the problems in the prior art, designs a perovskite single crystal X-ray detector with small ion migration and a manufacturing method thereof, prepares a cm-level MAPBR 3 perovskite single crystal by a space limitation and inverse temperature crystallization method, can directly grow single crystals on a substrate, and effectively solves the problems that: the X-ray detector has the advantages of integration mass production, high compatibility and stability, long service life and the like, and particularly has the characteristic of small ion migration. The X-ray detector is used for rapidly detecting X-rays at normal temperature, the current value of the X-ray detector is greatly changed under different X-ray doses, the sensitivity is high, the work is stable, and the detection can be directly carried out at room temperature; the preparation process is simple, the preparation cost is low, and the preparation process is pollution-free.
In order to achieve the purpose, the invention adopts the following scheme:
a perovskite single crystal X-ray detector with small ion migration is characterized in that perovskite single crystals in the X-ray detector are prepared by space limitation and inverse temperature crystallization methods and have centimeter-level MAPbBr3A perovskite single crystal;
a method for manufacturing an X-ray detector with small ion migration comprises the following steps:
stp 1: firstly, weighing MABr (purity is more than or equal to 99.9) with set weight9 percent) of the mixed solution, putting the mixed solution into a glass bottle, then injecting N, N-Dimethylformamide (DMF) solution with a set volume into the glass bottle, stirring the solution, and then weighing 0.707 to 1.101g of PbBr2(the purity is more than or equal to 99.9 percent) and putting the mixture into the glass bottle; then, the glass bottle is placed on a heating table at 60 ℃ to be stirred, so that the white powder in the glass bottle is completely dissolved until the solution is clear and transparent, and the precursor solution of the perovskite is obtained;
stp 2: manufacturing a limiting space, clamping a U-shaped die between two pieces of ITO conductive glass, and fixing the U-shaped die by using a high-temperature adhesive tape;
stp 3: and fixing the manufactured U-shaped grinding tool by using a clamp, then placing the U-shaped grinding tool on a heating table, extracting a certain amount of perovskite precursor solution by using an injector, and injecting the perovskite precursor solution into the U-shaped mould from the top of the U-shaped mould. Then heating by using a heating table, setting the initial temperature of the heating table to be 60 ℃, increasing the temperature by 5 ℃ every 15 minutes until the temperature reaches 90 ℃, increasing the temperature by 5 ℃ every 30 minutes until the temperature reaches 120 ℃ and keeping the temperature until the single crystal grows out, periodically replacing the solution in the U-shaped mould after the daughter crystal grows out in the U-shaped mould, and replacing half of the liquid in the U-shaped mould every half hour until MAPBBr is obtained3A perovskite single crystal;
stp 4: in the prepared MAPbBr3Preparing electrode on perovskite monocrystal, making MAPbBr-based3The perovskite monocrystal X-ray detector comprises the following steps: first, an electrode mask was placed on MAPbBr prepared as stp33Sputtering Au metal on the perovskite single crystal in sequence under argon atmosphere by using a direct current sputtering method, sputtering for 15s under the same sputtering power, and finally obtaining the MAPbBr-based metal3An X-ray detector for perovskite single crystal.
In stp1, the following are set:
the weight of MABr is 0.2-0.5 g, and the purity is more than or equal to 99.99%;
PbBr2the weight of the compound is 0.5-1.5 g, and the purity is more than or equal to 99.9%;
the volume of the N, N-Dimethylformamide (DMF) solution is 2-4 ml.
In stp2, the following are set: the spacing distance between the two ITO conductive glasses is 0.5 mm.
The principle of the invention is as follows: preparing centimeter-level MAPbBr by space limitation and inverse temperature crystallization3The perovskite single crystal reduces defect density, increases fluorescence lifetime, and inhibits ion migration.
The invention has the beneficial effects that:
(1) the invention prepares the MAPbBr with the centimeter grade by the methods of space limitation and inverse temperature crystallization3Perovskite single crystal, easy MEMS compatibility and integration.
(2) The invention reduces the defect density, prolongs the fluorescence life, inhibits the ion migration, has simple process and is easy for large-scale industrial production by regulating the molar ratio of the precursor solution.
Drawings
FIG. 1 is an XRD physical phase diagram of MAPbBr3 perovskite single crystal;
FIG. 2.1 is MAPbBr of example 13Defect density and carrier profile of the perovskite single crystal;
FIG. 2.2 MAPbBr of example 23Defect density and carrier profile of the perovskite single crystal;
FIG. 2.3 is MAPbBr of example 33Defect density and carrier profile of the perovskite single crystal;
FIG. 2.4 MAPbBr of example 43Defect density and carrier profile of the perovskite single crystal;
FIG. 3.1 is MAPbBr of example 13Hysteresis curves of the perovskite single crystals;
FIG. 3.2 MAPbBr of example 23Hysteresis curves of the perovskite single crystals;
FIG. 3.3 is MAPbBr of example 33Hysteresis curves of the perovskite single crystals;
FIG. 3.4 is MAPbBr of example 43Hysteresis curves of the perovskite single crystals;
FIG. 4.1 is MAPbBr of example 13I/t curve of perovskite single crystal;
FIG. 4.2 MAPbBr of example 23I/t curve of perovskite single crystal;
FIG. 4.3 is MAPbBr of example 33Of perovskite single crystalsAn I/t curve;
FIG. 4.4 is MAPbBr of example 43I/t curve of perovskite single crystal;
FIG. 5 is MAPbBr of example 33X-ray response of perovskite single crystal.
Detailed Description
The embodiments of the present invention will be further described with reference to the accompanying drawings, wherein the technical solutions of the present invention are described below in a clear and complete manner to make the objects, technical solutions and advantages of the present invention clearer, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to a manufacturing method of a perovskite single crystal X-ray detector with small ion migration, which is based on the following principle: preparation of centimeter-level MAPbBr by space limitation and inverse temperature crystallization3Perovskite single crystals reduce defect density, increase fluorescence lifetime and inhibit ion migration.
The X-ray detector prepared by the method is a centimeter-level MAPbBr prepared by the method based on space limitation and inverse temperature crystallization3The perovskite single crystal is easy to be compatible and integrated with MEMS, and the defect density is reduced, the fluorescence life is prolonged, and the ion migration is inhibited by adjusting and controlling the molar ratio of the precursor solution.
Specifically, the invention relates to a method for manufacturing an X-ray detector with small ion migration, which comprises the following steps:
stp 1: firstly weighing MABr (the purity is more than or equal to 99.99%) with set weight, putting the MABr into a 10mL glass bottle, then injecting N, N-Dimethylformamide (DMF) solution with set weight into the glass bottle, stirring, and then weighing PbBr with set weight2(purity is more than or equal to 99.9 percent) and put into a glass bottle filled with the solution. And (3) stirring the solution on a heating table set at 60 ℃ to completely dissolve the white powder medicine until the solution is in a clear and transparent state, thus obtaining the precursor solution of the perovskite.
stp 2: and manufacturing a limiting space, clamping the U-shaped die between two pieces of ITO conductive glass, and winding and binding the U-shaped die by using a high-temperature adhesive tape.
stp 3: fixing the manufactured U-shaped grinding tool by using a clamp, then placing the U-shaped grinding tool on a heating table, extracting a certain amount of precursor solution of the perovskite by using an injector, and injecting the precursor solution of the perovskite into the mold from the top of the mold. Heating was then started using a heating stage, the initial temperature of which was set at 60 ℃, and then increased by 5 ℃ every 15 minutes until the temperature reached 90 ℃, and then increased by 5 ℃ every 30 minutes until 120 ℃ and held until the single crystal grew out. When the seed crystal grows out of the mould, the solution in the mould is replaced periodically, namely: half of the liquid in the abrasive was replaced every half hour.
stp 4: in the prepared MAPbBr3Preparing electrode on perovskite monocrystal, making MAPbBr-based3The perovskite monocrystal X-ray detector comprises the following steps: first, an electrode mask was placed on MAPbBr prepared as stp33Sputtering Au metal on the perovskite single crystal in sequence under argon atmosphere by using a direct current sputtering method, sputtering for 15s under the same sputtering power, and finally obtaining the MAPbBr-based metal3An X-ray detector for perovskite single crystal.
In stp1, the following are set:
the weight of MABr is 0.2-0.5 g, and the purity is more than or equal to 99.99%;
PbBr2the weight of the compound is 0.5-1.5 g, and the purity is more than or equal to 99.9%;
the volume of the N, N-Dimethylformamide (DMF) solution is 2-4 ml.
In stp2, the following are set: the spacing distance between the two ITO conductive glasses is 0.5 mm.
The invention prepares the MAPbBr with the centimeter grade by the methods of space limitation and inverse temperature crystallization3The perovskite single crystal reduces defect density, prolongs fluorescence lifetime, and inhibits ion migration.
The following describes a method for manufacturing an X-ray detector with small ion mobility according to the present invention with four different embodiments:
example 1
stp 1: firstly weighing 0.336g MABr (purity is more than or equal to 99.99%) and putting into a 10mL glass bottle, then injecting 3mL N, N-Dimethylformamide (DMF) solution into the glass bottle and stirring, and then weighing 1.101g PbBr2(purity is more than or equal to 99.9 percent) and put into a glass bottle filled with the solution. And (3) stirring the solution on a heating table set at 60 ℃ to completely dissolve the white powder medicine until the solution is in a clear and transparent state, thus obtaining the precursor solution of the perovskite.
stp 2: make the restriction space, press from both sides the U type mould between two ITO conductive glass to twine with the high temperature sticky tape and tie up, set up: the spacing distance between the two ITO conductive glasses is 0.5 mm.
stp 3: fixing the manufactured U-shaped grinding tool by using a clamp, then placing the U-shaped grinding tool on a heating table, extracting a certain amount of precursor solution of the perovskite by using an injector, and injecting the precursor solution of the perovskite into the mold from the top of the mold. Heating was then started using a heating stage, the initial temperature of which was set at 60 ℃, then increased by 5 ℃ every 15 minutes until the temperature reached 90 ℃, and then increased by 5 ℃ every 30 minutes until 120 ℃ and held until the single crystal grew out. After the seed crystals are grown in the mold, the solution in the mold is periodically changed, and half of the liquid in the mold is changed every half hour.
stp 4: preparing an electrode on the prepared MAPbBr3 perovskite single crystal to prepare an X-ray detector based on the MAPbBr3 perovskite single crystal, wherein the steps are as follows: firstly, an electrode mask is placed on MAPbBr3 perovskite single crystal prepared according to stp3, Au metal is sputtered in sequence in an argon atmosphere by a direct-current sputtering method for 15s under the same sputtering power, and finally, the X-ray detector based on MAPbBr3 perovskite single crystal is obtained.
Example 2
stp 1: first, 0.336g of MABr (purity not less than 99.99%) is weighed and put into a 10mL glass bottle, then 3mL of N, N-Dimethylformamide (DMF) solution is injected into the glass bottle and stirred, and then 0.909g of PbBr is weighed2(purity is more than or equal to 99.9 percent) and thenInto a glass bottle containing the solution. And (3) stirring the solution on a heating table set at 60 ℃ to completely dissolve the white powder medicine until the solution is in a clear and transparent state, thus obtaining the precursor solution of the perovskite.
stp 2: make the restriction space, press from both sides the U type mould between two ITO conductive glass to twine with the high temperature sticky tape and tie up, set up: the spacing distance between the two ITO conductive glasses is 0.5 mm.
stp 3: fixing the manufactured U-shaped grinding tool by using a clamp, then placing the U-shaped grinding tool on a heating table, extracting a certain amount of precursor solution of the perovskite by using an injector, and injecting the precursor solution of the perovskite into the mold from the top of the mold. Heating was then started using a heating stage, the initial temperature of which was set at 60 ℃, then increased by 5 ℃ every 15 minutes until the temperature reached 90 ℃, and then increased by 5 ℃ every 30 minutes until 120 ℃ and held until the single crystal grew out. After the seed crystals are grown in the mold, the solution in the mold is periodically changed, and half of the liquid in the mold is changed every half hour.
stp 4: preparing an electrode on the prepared MAPbBr3 perovskite single crystal to prepare an X-ray detector based on the MAPbBr3 perovskite single crystal, wherein the steps are as follows: firstly, an electrode mask is placed on MAPbBr3 perovskite single crystal prepared according to stp3, Au metal is sputtered in sequence in an argon atmosphere by a direct-current sputtering method for 15s under the same sputtering power, and finally, the X-ray detector based on MAPbBr3 perovskite single crystal is obtained.
Example 3
stp 1: firstly weighing 0.336g MABr (purity is more than or equal to 99.99%) and putting into a 10mL glass bottle, then injecting 3mL N, N-Dimethylformamide (DMF) solution into the glass bottle and stirring, and then weighing 0.808g PbBr2(purity is more than or equal to 99.9 percent) and put into a glass bottle filled with the solution. And (3) stirring the solution on a heating table set at 60 ℃ to completely dissolve the white powder medicine until the solution is in a clear and transparent state, thus obtaining the precursor solution of the perovskite.
stp 2: make the restriction space, press from both sides the U type mould between two ITO conductive glass to twine with the high temperature sticky tape and tie up, set up: the spacing distance between the two ITO conductive glasses is 0.5 mm.
stp 3: fixing the manufactured U-shaped grinding tool by using a clamp, then placing the U-shaped grinding tool on a heating table, extracting a certain amount of precursor solution of the perovskite by using an injector, and injecting the precursor solution of the perovskite into the mold from the top of the mold. Heating was then started using a heating stage, the initial temperature of which was set at 60 ℃, then increased by 5 ℃ every 15 minutes until the temperature reached 90 ℃, and then increased by 5 ℃ every 30 minutes until 120 ℃ and held until the single crystal grew out. After the seed crystals are grown in the mold, the solution in the mold is periodically changed, and half of the liquid in the mold is changed every half hour.
stp 4: preparing an electrode on the prepared MAPbBr3 perovskite single crystal to prepare an X-ray detector based on the MAPbBr3 perovskite single crystal, wherein the steps are as follows: firstly, an electrode mask is placed on MAPbBr3 perovskite single crystal prepared according to stp3, Au metal is sputtered in sequence in an argon atmosphere by a direct-current sputtering method for 15s under the same sputtering power, and finally, the X-ray detector based on MAPbBr3 perovskite single crystal is obtained.
Example 4
stp 1: first, 0.336g of MABr (purity not less than 99.99%) was weighed and put in a 10mL glass bottle, then 3mL of N, N-Dimethylformamide (DMF) solution was poured into the glass bottle and stirred, and then 0.707g of PbBr was weighed2(purity is more than or equal to 99.9 percent) and put into a glass bottle filled with the solution. And (3) stirring the solution on a heating table set at 60 ℃ to completely dissolve the white powder medicine until the solution is in a clear and transparent state, thus obtaining the precursor solution of the perovskite.
stp 2: make the restriction space, press from both sides the U type mould between two ITO conductive glass to twine with the high temperature sticky tape and tie up, set up: the spacing distance between the two ITO conductive glasses is 0.5 mm.
stp 3: fixing the manufactured U-shaped grinding tool by using a clamp, then placing the U-shaped grinding tool on a heating table, extracting a certain amount of precursor solution of the perovskite by using an injector, and injecting the precursor solution of the perovskite into the mold from the top of the mold. Heating was then started using a heating stage, the initial temperature of which was set at 60 ℃, then increased by 5 ℃ every 15 minutes until the temperature reached 90 ℃, and then increased by 5 ℃ every 30 minutes until 120 ℃ and held until the single crystal grew out. After the seed crystals are grown in the mold, the solution in the mold is periodically changed, and half of the liquid in the mold is changed every half hour.
stp 4: preparing an electrode on the prepared MAPbBr3 perovskite single crystal to prepare an X-ray detector based on the MAPbBr3 perovskite single crystal, wherein the steps are as follows: firstly, an electrode mask is placed on MAPbBr3 perovskite single crystal prepared according to stp3, Au metal is sputtered in sequence in an argon atmosphere by a direct-current sputtering method, 15s are sputtered under the same sputtering power, and finally, the X-ray detector based on MAPbBr3 perovskite single crystal is obtained.
As shown in fig. 1, the XRD phase diagram of MAPbBr3 perovskite single crystal shows diffraction peaks corresponding to (100), (200) and (300) planes at 14.9, 30.1 and 45.6 for all samples. No diffraction peaks of other substances were present in the diffractogram, indicating MAPbBr3Has good crystallization property and high purity, and is a high-quality single crystal. As shown in FIG. 2.1, the defect density of the single crystal prepared in example 1 was 2.1X 1011cm-3And a carrier mobility of 18.7cm2V-1s-1As shown in FIG. 2.2, the defect density of the single crystal prepared in example 2 was 5.3X 1010cm-3And a carrier mobility of 35.6 cm2V-1s-1As shown in FIG. 2.3, the defect density of the single crystal prepared in example 3 was 3.385X 1010cm-3And a carrier mobility of 43.6 cm2V-1s-1As shown in FIG. 2.4, the defect density of the single crystal prepared in example 4 was 3.49X 1010cm-3And a carrier mobility of at most 26.8cm2V-1s-1By comparison, the single crystal prepared in example 3 has the lowest defect density and the highest carrier mobility, which is advantageous for the preparation of high performance devices. Perovskite crystal can be researched through hysteresis curve of deviceThe ion mobility and hysteresis curve in the bulk is a test that can reflect the degree of ion mobility of a single crystal, fig. 3.1 is an I/V scan curve of example 1, fig. 3.2 is an I/V scan curve of example 2, fig. 3.3 is an I/V scan curve of example 3, and fig. 3.4 is an I/V scan curve of example 4. The I/V curves have different degrees of deviation. The greater the degree of deviation, indicating a more severe ion mobility for the device, the scan curves of example 3 almost overlap, indicating a lower ion mobility for the device. FIG. 4.1 is an I/t curve under X-ray irradiation of example 1, FIG. 4.2 is an I/t curve under X-ray irradiation of example 2, FIG. 4.1 is an I/t curve under X-ray irradiation of example 3, and FIG. 4.1 is an I/t curve under X-ray irradiation of example 4. The current of example 3 does not fluctuate with time, which shows that the device has stable and reliable performance, and provides good reliability and stability for the future application of actual X-ray detection. FIG. 5 is an X-ray response graph of MAPbBr3 perovskite single crystal of example 3, as the X-ray is switched according to a certain frequency, the current of the device also shows rectangular change, the baseline of the device is not shifted, and the stability of the device is also proved.
The invention prepares centimeter-level MAPbBr by space limitation and inverse temperature crystallization3Perovskite single crystals, easy MEMS compatibility and integration; by regulating the molar ratio of the precursor solution, the defect density is reduced, the fluorescence lifetime is prolonged, the ion migration is inhibited, the process is simple, and the large-scale industrial production is easy to realize.

Claims (3)

1. A manufacturing method of a perovskite single crystal X-ray detector with small ion migration is characterized in that: the perovskite single crystal is MAPbBr with centimeter level3Perovskite single crystal, and is prepared by space limitation and inverse temperature crystallization; the manufacturing method comprises the following steps:
stp 1: firstly weighing MABr with set weight, putting the MABr into a glass bottle, then injecting N, N-Dimethylformamide (DMF) solution with set volume into the glass bottle, stirring, and then weighing PbBr with set weight2And putting the glass bottle into the glass bottle; then the glass is putPlacing the bottle on a heating table at 60 ℃ for stirring to completely dissolve the white powder in the glass bottle until the solution is clear and transparent, thus obtaining a precursor solution of perovskite;
stp 2: manufacturing a limiting space, clamping a U-shaped die between two pieces of ITO conductive glass, and fixing the U-shaped die by using a high-temperature adhesive tape;
stp 3: fixing the manufactured U-shaped grinding tool by using a clamp, then placing the U-shaped grinding tool on a heating table, extracting a certain amount of perovskite precursor solution by using an injector, injecting the perovskite precursor solution into the U-shaped mould from the top of the U-shaped mould,
heating with heating table set at 60 deg.C, increasing temperature by 5 deg.C every 15 min until 90 deg.C is reached, increasing temperature by 5 deg.C every 30 min until 120 deg.C until single crystal grows out, and changing half of liquid in U-shaped mold every half hour until MAPBBr is obtained3A perovskite single crystal;
stp 4: in the prepared MAPbBr3Preparing electrode on perovskite monocrystal, making MAPbBr-based3An X-ray detector of perovskite single crystal; the method comprises the following steps: first, an electrode mask was placed on MAPbBr prepared as stp33Sputtering Au metal on the perovskite single crystal in sequence under argon atmosphere by using a direct current sputtering method, sputtering for 15s under the same sputtering power, and finally obtaining the MAPbBr-based metal3An X-ray detector for perovskite single crystal.
2. The method for producing a perovskite single crystal X-ray detector with small ion migration according to claim 1, wherein: in stp1, the following are set:
the weight of MABr is 0.2-0.5 g, and the purity is more than or equal to 99.99%;
PbBr2the weight of the compound is 0.5-1.5 g, and the purity is more than or equal to 99.9%;
the volume of the N, N-Dimethylformamide (DMF) solution is 2-4 ml.
3. The method for producing a perovskite single crystal X-ray detector with small ion migration according to claim 1, wherein: in stp2, the following are set: the spacing distance between the two ITO conductive glasses is 0.5 mm.
CN202111361430.2A 2021-04-16 2021-11-17 Perovskite single crystal X-ray detector with small ion migration and manufacturing method Pending CN114361349A (en)

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CN115850089A (en) * 2022-11-29 2023-03-28 电子科技大学长三角研究院(湖州) MAPbBr with smooth surface 3 Preparation method and application of perovskite square block

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115850089A (en) * 2022-11-29 2023-03-28 电子科技大学长三角研究院(湖州) MAPbBr with smooth surface 3 Preparation method and application of perovskite square block

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