CN108539012B - All-inorganic perovskite resistive random access memory and preparation method thereof - Google Patents
All-inorganic perovskite resistive random access memory and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an all-inorganic perovskite resistive random access memory and a preparation method thereof. The memory structure sequentially comprises a bottom electrode, a resistance change layer and a top electrode from bottom to top. ITO as bottom electrode, CsPbBr3The thin film is used as a resistance change layer, and a metal Pt, Au or W is used as a top electrode. Preparation procedureTo convert CsPbBr3Dissolving the powder in a DMSO solution to prepare a precursor solution, spin-coating the precursor solution on an ITO bottom electrode by using a spin coater, then dropwise adding toluene as an anti-solvent to quickly crystallize a perovskite layer, and annealing at 100-150 ℃ for 10-30 min to obtain compact CsPbBr3A polycrystalline thin film. Then CsPbBr3And depositing a top electrode on the surface of the film. The resistance change layer of the memory is made of all-inorganic materials, the preparation process is simple, the cost is low, and the device shows excellent resistance change characteristics and air thermal stability by changing the heating temperature and the heating time.
Description
Technical Field
The invention relates to an all-inorganic perovskite resistive random access memory and a preparation method thereof, belonging to the technical field of inorganic materials and microelectronics.
Background
With the advent of the big data era, people have higher and higher requirements on information storage, the traditional flash memory technology is difficult to meet the requirements of high-density storage, and the development of a new nonvolatile memory becomes a research hotspot in the semiconductor industry. The resistive random access memory has the advantages of low power consumption, high storage density, high erasing speed, multi-value storage and the like, becomes a powerful competitor of the next-generation nonvolatile memory, and has wide application prospect.
The basic structure of the resistive random access memory comprises a top electrode, a bottom electrode and a middle resistive layer. The main working principle is that the resistance change layer can be reversibly changed between a high resistance state and a low resistance state by changing the voltage or current applied between the top electrode and the bottom electrode, and the resistance of the device can not be changed when the applied voltage or current is removed.
The organic-inorganic hybrid perovskite material has the characteristics of high light absorption efficiency, long carrier diffusion length and the like, and is widely applied to solar cells and light-emitting diodes. Meanwhile, the material shows an obvious resistance transformation effect in voltage and current response, is simple in preparation process and low in cost, and can be applied to a resistive random access memory. However, organic-inorganic hybrid perovskite materials are very sensitive to water and oxygen, and are easily decomposed in air, greatly affecting the stability of devices, thereby limiting the applications thereof.
In order to solve the problem of instability of organic-inorganic hybrid perovskites, pure inorganic perovskites have become a hot point of research. Since CsX (Cl, Br, I) has extremely low solubility in DMF and DMSO, the general preparation method can only obtain thinner CsPbBr3The film (less than 100nm) has a large number of holes and poor continuity; meanwhile, the boiling point of DMSO is high (189 ℃), the solvent cannot be completely removed during low-temperature preparation, secondary phases are easy to appear in the film, the quality of the film is reduced, and the performance of the device is influenced.
Disclosure of Invention
The invention aims to solve the problems or the defects and provides a preparation method and a test means of an all-inorganic perovskite resistive random access memory. The preparation cost is lower, the performance is more stable, and the scale production can be realized.
The present invention is thus achieved. An all-inorganic perovskite resistive random access memory sequentially comprises a bottom electrode, a resistive layer and a top electrode from bottom to top, wherein the bottom electrode is transparent conductive glass ITO (indium tin oxide), namely In doped with Sn2O3The film is 100-300 nm thick, rectangular and 500-2 cm long; the material of the resistance change layer is CsPbBr3The thickness of the resistance change layer is 150-200 nm, the resistance change layer is rectangular, and the side length of the resistance change layer is 500 mu m-2 cm; the top electrode is made of Pt, Au or W metal, the thickness of the top electrode is 50-100 nm, the top electrode is round or rectangular, and the diameter or the side length of the top electrode is 50-900 mu m.
The preparation method of the resistive random access memory comprises the following steps:
Performing ultrasonic treatment on an ITO substrate in deionized water, acetone and alcohol for 40min respectively, drying the ITO, attaching an insulating adhesive tape, and irradiating the ITO surface with ultraviolet light in a UV instrument for 30 min;
Preparing solution A, namely adding 10-30 mmol of PbBr2The powder is dissolved in aqueous HBr solution with 10-50% percent concentration and stirred at room temperatureTo PbBr2Completely dissolved and stirred at room temperature until PbBr2And completely dissolving. And preparing a solution B, dissolving 10-60 mmol CsBr powder in deionized water, and stirring at room temperature until CsBr is completely dissolved. And (3) rapidly injecting the solution B into the solution A by using an injector, wherein the injection time is controlled to be 9-10 s. Methanol is used as cleaning fluid, and CsPbBr is obtained after multiple cleaning and suction filtration3Powdering, and finally adding CsPbBr3Placing the powder in a glove box in an argon atmosphere, annealing for 20-40 min on a hot bench at 50-100 ℃, removing redundant methanol, and obtaining pure and dry CsPbBr3Powder;
Taking 0.5-1.4 g CsPbBr3Dissolving the powder in a DMSO solution, stirring for 10-12 h in the dark at room temperature, standing for 0.5-2 h, filtering by using a filter with the diameter of 0.22 mu m, removing large particles in the solution, and obtaining the colorless and transparent CsPbBr3A precursor liquid. Taking 50-120 mu L CsPbBr3And (3) spin-coating the precursor solution on the ITO surface in the step (1), wherein the rotating speed of a spin coater is set to be 3000 r/min-5000 r/min, and the time is 40-60 s. Dropwise adding 200-1000 mu L of anti-solvent when the solution is spin-coated for 15-25 s to quickly crystallize the perovskite layer, then annealing at 100-150 ℃ for 10-30 min to remove excess solvent to obtain compact CsPbBr3A polycrystalline thin film;
the antisolvent is toluene, chlorobenzene, diethyl ether or ethyl acetate.
CsPbBr in step 3 by magnetron sputtering or vacuum evaporation3The top electrode is deposited on the surface of the thin film, and has a circular or rectangular shape, a diameter or side length of 50-900 μm, and a thickness of 50-100 nm. Thus, the all-inorganic perovskite resistive random access memory is prepared.
Compared with the prior art, the invention has the advantages that:
(1) directly adding the synthesized CsPbBr3The powder is dissolved in DMSO to improve solubility, and anti-solvent is used to accelerate crystallization, so that compact CsPbBr can be obtained at low temperature3A film.
(2) The film preparation method is simple, convenient to operate and low in cost.
(3) The device has stable performance, a larger storage window and good cycle tolerance, and shows good anti-aging characteristic.
Drawings
FIG. 1 is a schematic diagram of a structure of an all-inorganic perovskite resistive random access memory
FIG. 2 CsPbBr in example 13Thin film XRD diffraction pattern
FIG. 3 CsPbBr in example 13Film surface SEM topography
FIG. 4 is a schematic current-voltage diagram of a resistive random access memory cell in embodiment 1
FIG. 5 test chart of cycle endurance of RRAM cell in example 1
FIG. 6 is a schematic current-voltage diagram of a resistive random access memory cell in embodiment 2
FIG. 7 test chart of cycle endurance of RRAM cell in example 2
FIG. 8 CsPbBr in example 33Film surface SEM topography
FIG. 9 distribution diagram of high and low resistance states at different times of heating at 90 ℃ in example 3
FIG. 10 distribution diagram of high and low resistance states at 90 ℃ for different times in example 4
Reference numerals: 1-ITO substrate, 2-resistance change layer, 3-top electrode
Detailed Description
The present invention will be described in further detail with reference to the following examples and drawings, but the present invention is not limited to the following examples.
As shown in fig. 1, the all-inorganic perovskite resistive random access memory of the invention sequentially comprises a bottom electrode, a resistive layer and a top electrode from bottom to top.
ITO is used as a bottom electrode material, the bottom electrode is square, the side length of the bottom electrode is 2cm, the thickness of the bottom electrode is 200nm, and CsPbBr is selected as a resistance change layer material3The shape of the glass is rectangular, the side length of the glass is 2cm, and the thickness of the glass is 200 nm.
Example 1:
Performing ultrasonic treatment on an ITO substrate in deionized water, acetone and alcohol for 40min respectively, drying the ITO, attaching an insulating adhesive tape, and irradiating the ITO surface with ultraviolet light in a UV instrument for 30 min;
Preparation of A solution, 10mmol of PbBr2The powder was dissolved in 30mL HBr solution at 48% water content and stirred at room temperature to PbBr2And completely dissolving. Solution B was prepared by dissolving 20mmol CsBr powder in 10mL deionized water and stirring at room temperature until CsBr was completely dissolved. And (3) rapidly injecting the solution B into the solution A by using an injector, wherein the injection time is controlled to be 9-10 s. Methanol is used as cleaning fluid, and CsPbBr is obtained after multiple cleaning and suction filtration3Powdering, and finally adding CsPbBr3Annealing the powder at 100 deg.C for 30min in argon atmosphere to remove excessive methanol to obtain pure and dry CsPbBr3Powder;
1.4g CsPbBr was taken3Dissolving the powder in 2mL DMSO solution, stirring at room temperature in dark for 12h, standing for 30min, filtering with 0.22 μm diameter filter, removing large particles in the solution to obtain colorless transparent CsPbBr3A precursor liquid. 80 μ L of CsPbBr was taken3And (3) spin-coating the precursor solution on the ITO surface in the step (1), wherein the rotating speed of a spin coater is set to be 4000r/min, and the time is 60 s. Dripping 500 mu L of toluene on the surface of the rotating ITO vertically at a constant speed when the solution is spun for 15s, then annealing for 15min at the temperature of 100 ℃, removing the redundant solvent to obtain CsPbBr3A polycrystalline thin film;
Placing the substrate in the step 3 in an evaporation coating machine, and using a mask in CsPbBr3The top electrode is deposited on the surface of the film, the diameter is 900 μm, and the thickness is 100 nm. Thus, the all-inorganic perovskite resistive random access memory is prepared;
step 5, removing the insulating adhesive tape and testing the performance
And (3) carrying out a voltage-current test and a cycle endurance test on the sample by using a semiconductor parameter analyzer at room temperature.
Example 2:
Performing ultrasonic treatment on an ITO substrate in deionized water, acetone and alcohol for 40min respectively, drying the ITO, attaching an insulating adhesive tape, and irradiating the ITO surface with ultraviolet light in a UV instrument for 30 min;
Preparation of A solution, 10mmol of PbBr2The powder was dissolved in 30mL HBr solution at 48% water content and stirred at room temperature to PbBr2And completely dissolving. Solution B was prepared by dissolving 20mmol CsBr powder in 10mL deionized water and stirring at room temperature until CsBr was completely dissolved. And (3) rapidly injecting the solution B into the solution A by using an injector, wherein the injection time is controlled to be 9-10 s. Methanol is used as cleaning fluid, and CsPbBr is obtained after multiple cleaning and suction filtration3Powdering, and finally adding CsPbBr3Annealing the powder at 100 deg.C for 30min in argon atmosphere to remove excessive methanol to obtain pure and dry CsPbBr3Powder;
1.4g CsPbBr was taken3Dissolving the powder in 2mL DMSO solution, stirring at room temperature in dark for 12h, standing for 30min, filtering with 0.22 μm diameter filter, removing large particles in the solution to obtain colorless transparent CsPbBr3A precursor liquid. 80 μ L of CsPbBr was taken3And (3) spin-coating the precursor solution on the ITO surface in the step (1), wherein the rotating speed of a spin coater is set to be 4000r/min, and the time is 60 s. Dripping 500 mu L of toluene on the surface of the rotating ITO vertically at a constant speed when the temperature is 25s by spin coating, then annealing for 15min at the temperature of 100 ℃, removing the redundant solvent to obtain CsPbBr3A polycrystalline thin film;
Placing the substrate in the step 3 in an evaporation coating machine, and using a mask in CsPbBr3The top electrode is deposited on the surface of the film, the diameter is 900 μm, and the thickness is 100 nm. Thus, the all-inorganic perovskite resistive random access memory is prepared;
step 5, removing the insulating adhesive tape and testing the performance
And (3) carrying out a voltage-current test and a cycle endurance test on the sample by using a semiconductor parameter analyzer at room temperature.
Example 3:
Performing ultrasonic treatment on an ITO substrate in deionized water, acetone and alcohol for 40min respectively, drying the ITO, attaching an insulating adhesive tape, and irradiating the ITO surface with ultraviolet light in a UV instrument for 30 min;
Preparation of A solution, 10mmol of PbBr2The powder was dissolved in 30mL HBr solution at 48% water content and stirred at room temperature to PbBr2And completely dissolving. Solution B was prepared by dissolving 20mmol CsBr powder in 10mL deionized water and stirring at room temperature until CsBr was completely dissolved. And (3) rapidly injecting the solution B into the solution A by using an injector, wherein the injection time is controlled to be 9-10 s. Methanol is used as cleaning fluid, and CsPbBr is obtained after multiple cleaning and suction filtration3Powdering, and finally adding CsPbBr3Annealing the powder at 100 deg.C for 30min in argon atmosphere to remove excessive methanol to obtain pure and dry CsPbBr3Powder;
1.4g CsPbBr was taken3Dissolving the powder in 2mL DMSO solution, stirring at room temperature in dark for 12h, standing for 30min, filtering with 0.22 μm diameter filter, removing large particles in the solution to obtain colorless transparent CsPbBr3A precursor liquid. 80 μ L of CsPbBr was taken3And (3) spin-coating the precursor solution on the ITO surface in the step (1), wherein the rotating speed of a spin coater is set to be 4000r/min, and the time is 60 s. Dripping 500 μ L chlorobenzene on the surface of the rotating ITO at uniform speed vertically when the solution is spin-coated for 15s, then annealing for 15min at 100 ℃, removing the redundant solvent to obtain CsPbBr3A polycrystalline thin film;
Placing the substrate in the step 3 in an evaporation coating machine, and using a mask in CsPbBr3The top electrode is deposited on the surface of the film, the diameter is 900 μm, and the thickness is 100 nm. Thus, the all-inorganic perovskite resistive random access memory is prepared;
step 5, removing the insulating adhesive tape and testing the performance
And (3) placing the sample on a 90 ℃ hot stage to be heated for 0min, 30min, 60min and 90min respectively, and testing and analyzing the sample by using a semiconductor parameter analyzer to obtain high-low resistance state distribution corresponding to different heating times.
Example 4:
Performing ultrasonic treatment on an ITO substrate in deionized water, acetone and alcohol for 40min respectively, drying the ITO, attaching an insulating adhesive tape, and irradiating the ITO surface with ultraviolet light in a UV instrument for 30 min;
Preparation of A solution, 10mmol of PbBr2The powder was dissolved in 30mL HBr solution at 48% water content and stirred at room temperature to PbBr2And completely dissolving. Solution B was prepared by dissolving 20mmol CsBr powder in 10mL deionized water and stirring at room temperature until CsBr was completely dissolved. And (3) rapidly injecting the solution B into the solution A by using an injector, wherein the injection time is controlled to be 9-10 s. Methanol is used as cleaning fluid, and CsPbBr is obtained after multiple cleaning and suction filtration3Powdering, and finally adding CsPbBr3Annealing the powder at 100 deg.C for 30min in argon atmosphere to remove excessive methanol to obtain pure and dry CsPbBr3Powder;
1.4g CsPbBr was taken3Dissolving the powder in 2mL DMSO solution, stirring at room temperature in dark for 12h, standing for 30min, filtering with 0.22 μm diameter filter, removing large particles in the solution to obtain colorless transparent CsPbBr3A precursor liquid. 80 μ L of CsPbBr was taken3And (3) spin-coating the precursor solution on the ITO surface in the step (1), wherein the rotating speed of a spin coater is set to be 4000r/min, and the time is 60 s. Dripping 500 μ L chlorobenzene on the surface of the rotating ITO at uniform speed vertically when the temperature is 25s by spin coating, then annealing for 15min at 100 ℃, removing the redundant solvent to obtain CsPbBr3A polycrystalline thin film;
Placing the substrate in the step 3 in an evaporation coating machine, and using a mask in CsPbBr3The top electrode is deposited on the surface of the film, the diameter is 900 μm, and the thickness is 100 nm. To this end, the total ofA perovskite resistive random access memory;
step 5, removing the insulating adhesive tape and testing the performance
And (3) placing the sample on a 90 ℃ hot stage to be heated for 0min, 30min, 60min and 90min respectively, and testing and analyzing the sample by using a semiconductor parameter analyzer to obtain high-low resistance state distribution corresponding to different heating times.
Claims (1)
1. The full-inorganic perovskite resistive random access memory sequentially comprises a bottom electrode, a resistive layer and a top electrode from bottom to top, and is characterized In that the bottom electrode is transparent conductive glass ITO (indium tin oxide), namely In doped with Sn2O3The film is 100-300 nm thick, rectangular and 500-2 cm long; the material of the resistance change layer is CsPbBr3The thickness of the resistance change layer is 150-200 nm, the resistance change layer is rectangular, and the side length of the resistance change layer is 500 mu m-2 cm; the top electrode is made of Pt, Au or W metal, the thickness of the top electrode is 50-100 nm, the top electrode is in a round or rectangular shape, the diameter or side length of the top electrode is 50-900 mu m, and the top electrode is compact CsPbBr3The film is prepared by a spin-coating method;
the all-inorganic perovskite resistive random access memory is prepared by the following steps:
1) cleaning the ITO substrate
Performing ultrasonic treatment on an ITO substrate in deionized water, acetone and alcohol for 40min respectively, drying the ITO, attaching an insulating adhesive tape, and irradiating the ITO surface with ultraviolet light in a UV instrument for 30 min;
2) preparation of fully inorganic CsPbBr3Powder of
Preparing solution A, namely adding 10-30 mmol of PbBr2The powder is dissolved in HBr aqueous solution with the percentage concentration of 10 percent to 50 percent and stirred at room temperature until PbBr is obtained2Completely dissolving; preparing a solution B, dissolving 10-60 mmol CsBr powder in deionized water, and stirring at room temperature until CsBr is completely dissolved; rapidly injecting the solution B into the solution A by using an injector, wherein the injection time is controlled within a certain range; methanol is used as cleaning fluid, and CsPbBr is obtained after multiple cleaning and suction filtration3Powdering, and finally adding CsPbBr3Placing the powder in a glove box under argon atmosphere, annealing on a heating table at appropriate temperature for a period of time, and removingExcess methanol to obtain pure and dry CsPbBr3Powder;
3) preparation of dense CsPbBr3Polycrystalline thin film
Taking 0.5-1.4 g CsPbBr3Dissolving the powder in a DMSO solution, stirring for 10-12 h in the dark at room temperature, standing for 0.5-2 h, filtering by using a filter with the diameter of 0.22 mu m, removing large particles in the solution, and obtaining the colorless and transparent CsPbBr3A precursor solution; taking 50-120 mu L CsPbBr3Spin-coating the precursor solution on the ITO surface in the step 1, setting the rotating speed of a spin coater to be 3000 r/min-5000 r/min for 40-60 s, dropwise adding 200-1000 mu L of an anti-solvent when the spin coating is carried out for 15-25 s to quickly crystallize a perovskite layer, annealing for 10-30 min at the temperature of 100-150 ℃, removing the redundant solvent to obtain compact CsPbBr3A polycrystalline thin film;
the anti-solvent is toluene, chlorobenzene, diethyl ether or ethyl acetate;
4) preparing the top electrode
CsPbBr in step 3 by magnetron sputtering or vacuum evaporation3Depositing a top electrode on the surface of the film, wherein the top electrode is round or rectangular, the diameter or side length of the top electrode is 50-900 micrometers, and the thickness of the top electrode is 50-100 nm;
thus, the all-inorganic perovskite resistive random access memory is prepared.
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| CN110690302B (en) * | 2019-08-19 | 2021-08-17 | 五邑大学 | CsPbBr3Thin film, preparation method thereof and device |
| CN110660912A (en) * | 2019-09-19 | 2020-01-07 | 深圳第三代半导体研究院 | Preparation method of flexible resistive random access memory device based on perovskite |
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