CN110797456A - Lead-free double perovskite-based electric storage device and preparation method thereof - Google Patents
Lead-free double perovskite-based electric storage device and preparation method thereof Download PDFInfo
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- CN110797456A CN110797456A CN201910996312.5A CN201910996312A CN110797456A CN 110797456 A CN110797456 A CN 110797456A CN 201910996312 A CN201910996312 A CN 201910996312A CN 110797456 A CN110797456 A CN 110797456A
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- H10N70/00—Solid-state devices without a potential-jump barrier or surface barrier, and specially adapted for rectifying, amplifying, oscillating or switching
- H10N70/011—Manufacture or treatment of multistable switching devices
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Abstract
The invention discloses an electric storage device based on lead-free double perovskite and a preparation method thereof; lead-free double perovskite Cs2AgBiBr6Dissolving the powder in a DMSO solvent, and preparing a yellow lead-free double perovskite solution after full oscillation; coating a lead-free double perovskite solution on a substrate to prepare an active layer; then preparing an electrode on the active layer to obtain the lead-free double perovskite-based Cs2AgBiBr6The electrical storage device of (1). The invention utilizes inorganic metal halide to form a lead-free double perovskite material through coordination to prepare the electric storage device with a sandwich structure, successfully realizes the electric storage behavior, has simple preparation process, good stability of the electric storage behavior, strong environmental and high temperature tolerance and no toxicity of the material.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a lead-free double perovskite-based material Cs2AgBiBr6An electrical memory device and a method of making the same.
Background
With the rapid development of modern information technology, human society has entered the era of information explosion, the information amount has increased explosively, the traditional storage technology cannot meet the storage requirement of such a large amount of information, people urgently need a novel storage technology with ultrahigh-density information storage capacity, and under such a background, the electric storage technology is developed, and an electric storage device consists of an upper electrode, a lower electrode and a middle active layer. Under the action of an electric field, the electric storage device can show different conduction states, so that the electric storage device has an information storage function. The selective range of the active layer material is very wide, and the possibility is provided for realizing the memory with excellent performance. However, the stability of the current storage materials to the environment and high temperature is poor, which is a great obstacle to the practical application of the electrical storage technology, so that a new material solution is urgently needed to solve the problems of the current electrical storage technology.
Disclosure of Invention
Aiming at the problems of high toxicity, sensitive humidity, poor stability in environment and high temperature and the like of the conventional perovskite electric storage material, the invention discloses a lead-free double perovskite-based material Cs2AgBiBr6The electric storage device and the preparation method thereof have the advantages of simple preparation process, good stability of electric storage behavior, strong environmental and high temperature tolerance, and nontoxic materials, and have important significance for the industrial and practical use of the electric storage technology.
The invention adopts the following technical scheme that the preparation method of the lead-free double perovskite-based electric storage device comprises the following steps: coating a lead-free double perovskite organic solvent solution on a substrate, and preparing an electric storage material layer by heat treatment; and then preparing an electrode on the electric storage material layer to obtain the electric storage device based on the lead-free double perovskite.
A lead-free double perovskite electricity storage material is prepared by the following steps: coating a lead-free double perovskite organic solvent solution on a substrate, and performing heat treatment to prepare the electric storage material.
A lead-free double perovskite solution for an electric memory device is prepared by dissolving cesium salt, silver salt and bismuth salt in hydrobromic acid aqueous solution, and heating for reaction to obtain lead-free double perovskite; and dissolving the lead-free double perovskite into an organic solvent to obtain a lead-free double perovskite solution for the electric storage device.
The invention also discloses the application of the lead-free double perovskite in the preparation of an electric storage device; or the use of a lead-free double perovskite material as an electrical storage material.
In the present invention, the lead-free double perovskite is Cs2AgBiBr6(ii) a Dissolving cesium salt, silver salt and bismuth salt into hydrobromic acid aqueous solution, and heating for reaction to obtain lead-free double perovskite; preferably, the cesium salt is cesium bromide, the silver salt is silver bromide, and the bismuth salt is bismuth bromide; the concentration of the hydrobromic acid aqueous solution is 45-50 wt%; the heating reaction is carried out at the temperature of 110-130 ℃ for 0.8-1.2 hours; and after the heating reaction is finished, cooling to room temperature under the condition of keeping out of the sun, then carrying out reduced pressure filtration, washing with absolute ethyl alcohol, and finally drying under the protection of nitrogen to obtain the lead-free double perovskite. For example, cesium bromide, silver bromide and bismuth bromide are dissolved in 46wt% hydrobromic acid aqueous solution, heated to 120 ℃ for reaction for 1 hour, then the solution is cooled to room temperature under the condition of keeping out of the sun, filtered under reduced pressure, filter cake is washed with absolute ethyl alcohol for three times, and then dried for 6 hours at 60 ℃ under the protection of nitrogen, so that the lead-free double perovskite Cs is obtained2AgBiBr6。
In the present invention, the heat treatment is carried out at 280 ℃ for 5 minutes; coating the lead-free double perovskite organic solvent solution on a substrate by adopting spin coating, wherein the spin coating speed is 3000-5000 r/min, the time is 40-60 s, preferably the spin coating speed is 500 r/min, the spin coating time is 5s, and then the spin coating time is 5000 r/min and 40 s; the thickness of the electric storage material layer is 150-250 nm. Preferably, in the lead-free double perovskite organic solvent solution, the concentration of the lead-free double perovskite is 0.5 mmol/L, and the organic solvent is DMSO; lead-free double perovskite Cs2AgBiBr6The powder is dissolved in an organic solvent, heated to 50 ℃, and vibrated to obtain a yellow lead-free double perovskite solution, so that the double perovskite material is completely dissolved and is used for an electric storage device. The first low-speed spin coating is to uniformly distribute the solution on the substrate, and the second high-speed spin coating is to remove the excess solution.
In the invention, an evaporation method is adopted to prepare an electrode on an active layer; the vapor deposition conditions were 5X 10-4The vapor deposition rate is 1 Å/s under the Pa vacuum condition, and the thickness of the electrode is 100-200 nm.
In the invention, after a lead-free double perovskite organic solvent solution is coated on a substrate, the substrate is treated for 2min under the condition of reduced pressure, then the substrate is placed on a heating table, and annealing is carried out for 5 min under the condition of 280 ℃ to prepare an electric storage material layer; the substrate is ITO glass; the thickness of the electric storage material layer is 150-250 nm.
The lead-free double perovskite material is formed by utilizing the inorganic metal halide through coordination, the electric storage device with the sandwich structure is prepared, the electric storage behavior is successfully realized, the preparation process is simple, the stability of the electric storage behavior is good, the environment and high temperature tolerance is strong, the material is non-toxic, and the problems of high toxicity, humidity sensitivity, poor environment and high temperature stability and the like of the conventional electric storage device based on the perovskite material are solved.
Compared with the prior art, the invention using the technical scheme has the following advantages:
(1) the invention utilizes lead-free double perovskite material Cs2AgBiBr6As an active layer, a series of sandwich type electric storage devices are prepared, and the active layer is made of a non-toxic material and has more practical application significance;
(2) the lead-free double perovskite-based electric storage device can be prepared in an air environment, and compared with the traditional perovskite material which needs to be prepared under the protection of inert gas, the technical scheme is simpler and more convenient to operate and lower in cost;
(3) compared with the traditional device, the lead-free double perovskite-based electric storage device has better environmental and high-temperature stability, and has great significance for the practicability of the perovskite-based electric storage device.
Drawings
FIG. 1 is a schematic structural diagram of an electrical storage device based on lead-free double perovskite, which includes a glass substrate, an ITO bottom electrode, a lead-free double perovskite active layer and a gold top electrode from bottom to top;
FIG. 2 is a diagram showing the results of testing the storage performance of an electrical storage device based on lead-free double perovskite according to an embodiment, wherein the device shows a binary Flash type electrical storage behavior, and the electrical storage performance of the device is still maintained after 1000 erasing and writing cycles, so that the device shows better stability;
FIG. 3 is a graph of the memory performance of the lead-free double perovskite-based electrical memory device of the second embodiment under different conditions, (a) the electrical memory behavior of the device after being left in an atmospheric environment for a period of time, the device still maintaining good memory behavior after 25 days; (b) the storage behavior of the device under different humidity environments is shown, and the storage performance of the device is kept stable in the variation range of the relative humidity from 10% to 80%; (c) the storage behaviors of the device under different temperature environments are shown, and the storage performance of the device can still be maintained in the temperature range from 303K to 473K; (d) the figure shows the storage behavior of the device after the device is burned for 10 s in an alcohol lamp, and the performance is stable;
FIG. 4 is an X-ray diffraction diagram of the lead-free double perovskite-based electrical storage device of the second embodiment under different external condition treatments, wherein the lead-free double perovskite-based electrical storage device is stable after the device is placed in the environment for 31 days, treated at 90% relative humidity for 1 h, heated at 100 ℃ for 1 h and burned in an alcohol lamp for 10 s;
FIG. 5 shows the results of the ultraviolet-visible spectrum test of the lead-free double perovskite-based electrical storage device of the third embodiment, wherein the band gap of the lead-free double perovskite-based electrical storage device is 2.13 eV;
FIG. 6 is an SEM cross-sectional view of a lead-free double perovskite-based electrical storage device according to a second embodiment;
FIG. 7 shows tribromoplumbate methylamine (MAPbBr) based on perovskite material3) And cesium tribromide plumbate (CsPbBr)3) The prepared electric storage device has electric storage behavior under different humidity environments.
Detailed Description
The technical solutions of the present invention will be further described with reference to the accompanying drawings and specific embodiments. Unless otherwise indicated, reagents, materials, instruments and the like used in the following examples are commercially available.
Example one
Cesium bromide (425.6 mg, 2 mmol), silver bromide (187.8 mg, 1 mmol), bismuth bromide (448.7 mg, 1 mmol) were dissolved in 46wt% aqueous hydrobromic acid (30 mL) and heated to 120 ℃ for 1 hour. Then naturally cooling the solution to room temperature in the dark, filtering under reduced pressure, and using anhydrous ethyl acetate to filter cakesWashing with alcohol for three times, and drying at 60 ℃ for 6 hours under the protection of nitrogen to obtain the lead-free double perovskite Cs2AgBiBr6。
Mixing the above Cs2AgBiBr6(1063 mg, 1 mmol) was dissolved in DMSO (2 mL), and the solution was heated to 50 ℃ and shaken to obtain yellow lead-free double perovskite Cs2AgBiBr6And (3) solution.
The structure of an electric storage device based on lead-free double perovskite is shown in figure 1, the device is basically divided into three layers, namely an ITO glass substrate layer, an electric storage material layer and a gold electrode layer from bottom to top, and the preparation method comprises the following specific steps:
1. in an ultrasonic cleaning instrument, sequentially cleaning an ITO glass substrate by using deionized water, acetone and absolute ethyl alcohol;
2. (ii) by spin coating Cs2AgBiBr6Spin-coating the solution on an ITO glass substrate, carrying out reduced pressure treatment for 2 minutes, and then annealing at 280 ℃ for 5 minutes to form an electric storage material layer with the thickness of 200 nm; the spin coating conditions were as follows: the solution is dripped on a substrate, and the rotating speeds of the two sections are respectively as follows: 500 r/min for 5s, 5000 r/min for 40 s.
3. Evaporating a gold electrode on the electric storage material layer until the thickness of the gold electrode reaches 200 nm to obtain an electric storage device based on the lead-free double perovskite; the evaporation conditions were as follows: at 5X 10-4The vapor deposition rate under Pa vacuum was 1 Å/s.
Fig. 2 is a result diagram of a test result of the storage performance of the lead-free double perovskite-based electric storage device, the device shows a binary Flash type electric storage behavior, and after the device is erased and written for 1000 times, the electric storage performance is still maintained, so that better stability is shown.
The lead-free double perovskite-based electric storage device has good environmental qualitative performance, and still shows stable storage performance after being placed in an atmospheric environment for 25 days; the high-temperature stability is good, and the storage performance is still kept when the temperature is heated to 463K; the storage device is insensitive to humidity, and can show stable storage performance in an environment with the relative humidity range of 10% -80%. Fig. 3 shows the storage performance of the lead-free double perovskite-based electric storage device under different conditions, (a) shows the electric storage behavior of the device after being placed in an atmospheric environment for a period of time, and the device still maintains good storage behavior after 25 days; (b) the storage behavior of the device under different humidity environments is shown, and the storage performance of the device is kept stable in the variation range of the relative humidity from 10% to 80%; (c) the storage behaviors of the device under different temperature environments are shown, and the storage performance of the device can still be maintained in the temperature range from 303K to 473K; (d) the figure shows the storage behavior of the device after burning for 10 s in an alcohol burner, and the performance is stable.
FIG. 4 is an X-ray diffraction diagram of the lead-free double perovskite electric storage device under different external condition treatment conditions, wherein after the device is placed in the environment for 31 days, the device is treated with 90% relative humidity for 1 h, heated at 100 ℃ for 1 h and burnt by an alcohol lamp for 10 s, the lead-free double perovskite material Cs2AgBiBr6All remain stable.
FIG. 5 shows the result of the above-mentioned UV-visible spectrum test of the lead-free double perovskite-based electrical storage device, the lead-free double perovskite material Cs2AgBiBr6The band gap is 2.13 eV.
Fig. 6 is an SEM cross-sectional view of the above lead-free double perovskite-based electrical memory device.
FIG. 7 shows tribromoplumbate methylamine (MAPbBr) based on perovskite material3) And cesium tribromide plumbate (CsPbBr)3) The prepared electric storage device has electric storage behaviors under different humidity environments (except different perovskite materials, the rest of the electric storage device is consistent with the device of the invention); the device can not work normally under the environment with the humidity higher than 60%, and the storage performance is damaged, which indicates that the device can not work under the high-humidity environment.
The invention utilizes lead-free double perovskite-based material Cs2AgBiBr6The prepared electric storage device with the sandwich structure successfully realizes the electric storage behavior of a binary Flash type, has simple preparation process, high cyclic erasing frequency of 1000 times and strong tolerance to environment, high temperature and moderate degree, and solves the problems of high toxicity, humidity sensitivity and environmental and high-temperature stability of the conventional perovskite electric storage devicePoor, etc.; the lead-free double perovskite material has excellent performance and can be compounded with other materials for use; by utilizing the lead-free double perovskite material Cs2AgBiBr6The electric storage device has extremely high application value with the electric storage device prepared by combining the existing shell and the electrode lead in a conventional mode.
Claims (10)
1. Use of a lead-free double perovskite for the preparation of an electrical storage device; or the use of a lead-free double perovskite material as an electrical storage material.
2. The use according to claim 1, wherein the lead-free double perovskite is prepared by dissolving a cesium salt, a silver salt, and a bismuth salt in an aqueous hydrobromic acid solution, and heating to react the resulting solution to obtain the lead-free double perovskite.
3. An electrical storage device based on lead-free double perovskite, characterized in that the preparation method of the electrical storage device based on lead-free double perovskite comprises the following steps: coating a lead-free double perovskite organic solvent solution on a substrate, and preparing an electric storage material layer by heat treatment; and then preparing an electrode on the electric storage material layer to obtain the electric storage device based on the lead-free double perovskite.
4. The lead-free double perovskite-based electrical storage device as claimed in claim 3, wherein the lead-free double perovskite is prepared by dissolving cesium salt, silver salt and bismuth salt in hydrobromic acid aqueous solution, and heating to react to obtain the lead-free double perovskite.
5. The lead-free double perovskite-based electrical storage device of claim 4, wherein the cesium salt is cesium bromide, the silver salt is silver bromide, and the bismuth salt is bismuth bromide; the concentration of the hydrobromic acid aqueous solution is 45-50 wt%; the heating reaction is carried out at the temperature of 110-130 ℃ for 0.8-1.2 hours; and after the heating reaction is finished, cooling to room temperature under the condition of keeping out of the sun, then carrying out reduced pressure filtration, washing a filter cake with absolute ethyl alcohol, and drying under the protection of nitrogen to obtain the lead-free double perovskite.
6. The lead-free double perovskite-based electrical storage device as defined in claim 3, wherein the heat treatment is heating at 280 ℃ for 5 minutes; coating the lead-free double perovskite organic solvent solution on a substrate by adopting spin coating, wherein the spin coating speed is 3000-5000 r/min, and the time is 40-60 s; the thickness of the electric storage material layer is 150-250 nm.
7. The lead-free double perovskite-based electrical storage material is characterized in that the preparation method of the lead-free double perovskite-based electrical storage material comprises the following steps: coating a lead-free double perovskite organic solvent solution on a substrate, and performing heat treatment to prepare the electric storage material.
8. A lead-free double perovskite solution for an electric storage device is characterized in that the preparation method of the lead-free double perovskite solution for the electric storage device comprises the steps of dissolving cesium salt, silver salt and bismuth salt in hydrobromic acid aqueous solution, and heating for reaction to obtain the lead-free double perovskite; and dissolving the lead-free double perovskite into an organic solvent to obtain a lead-free double perovskite solution for the electric storage device.
9. A lead-free double perovskite material is characterized in that the preparation method of the lead-free double perovskite material is that cesium salt, silver salt and bismuth salt are dissolved in hydrobromic acid water solution and heated for reaction to obtain the lead-free double perovskite.
10. A preparation method of an electric storage device based on lead-free double perovskite is characterized by comprising the following steps: coating a lead-free double perovskite organic solvent solution on a substrate, and preparing an electric storage material layer by heat treatment; and then preparing an electrode on the electric storage material layer to obtain the electric storage device based on the lead-free double perovskite.
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| CN114751447B (en) * | 2022-04-13 | 2023-09-19 | 滨州裕能化工有限公司 | Cs (cell lines) 2 TiBr 6 Process for preparing powder |
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Application publication date: 20200214 |