CN113540386B - Perovskite light-emitting diode with GaN semiconductor material as electron transport layer and preparation method thereof - Google Patents
Perovskite light-emitting diode with GaN semiconductor material as electron transport layer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a perovskite light-emitting diode with a GaN semiconductor material as an electron transport layer and a preparation method thereof. The invention adopts different types of GaN semiconductor materials as the electron transport layer of the perovskite light emitting diode. In addition, the two-dimensional GaN quantum size effect is obvious, and the conductive characteristic is better. With the increase of the number of layers of the two-dimensional GaN, the reflection characteristic to light is better and better. The GaN with the porous structure can be in full contact with the perovskite material, and the maximum photogenerated charge separation and charge injection are ensured. Therefore, GaN material is a suitable choice as an electron transport layer of the light emitting diode, which can improve the quantum efficiency of the device.
Description
Technical Field
The invention relates to a perovskite light-emitting diode with a GaN semiconductor material as an electron transport layer and a preparation method thereof, belonging to the technical field of semiconductor devices.
Background
In the prior art, halogenated lead perovskite AMX3(wherein A ═ CH)3NH3 +，CH(NH2 ) 2 +，Cs+；M＝Pb2+，Sn2+；X＝I-，Br-，Cl-) Due to its high External Quantum Efficiency (EQE), it has evolved from below 1% to 20%, color tunable properties, narrow-band emission, and easy solution preparation, etc., and has attracted global attention in the field of low-cost illumination and high-resolution displays. Perovskite-type light emitting diodes (PeLEDs) generally consist of anode/Hole Transport Layer (HTL)/perovskite emission layer (EML)/Electron Transport Layer (ETL)/cathode, and interface engineering is one of the most critical strategies to improve device performance, particularly at the cathode/ETL interface. This is because there is always an energy level mismatch between the ETL and the electrode, which affects the balance of electron and hole injection, resulting in a decrease in the quantum efficiency of the device.
ETLs are not only specifically designed to extract photocurrent, but also need to exhibit chemical and physical properties, such as chemical durability, interface properties, thermal/electrical conductivity, band alignment, optical properties (e.g., refractive index and light transmittance), commensurate with other peled structures. TiO 22ZnO, PEDOT are the initial materials for ETL, however, these materials have several disadvantages, such as poor electron transportRate, chemical instability in acid-base solutions, reactivity with perovskite layers, difficulty in adjusting band structure, and the like.
Gallium nitride (GaN) has excellent optical and electrical properties, a direct band gap (Eg-3.4 eV), a transmittance exceeding 82% of the entire visible wavelength, high electron mobility, and the like. In addition, the thermal, mechanical, and chemical stability of GaN has enabled practical use of Light Emitting Diodes (LEDs), Laser Diodes (LDs), and Photodetectors (PDs). As the dimensionality decreases, the energy band of two-dimensional GaN widens. The two-dimensional GaN quantum size effect is obvious, and the conductive characteristic is better. With the increase of the number of layers of the two-dimensional GaN, the reflection characteristic to light is better and better. Besides the advantages of the single crystal material, the porous GaN single crystal material has the following potential outstanding advantages: (1) the porous structure is beneficial to full contact between GaN and perovskite materials, and can ensure the generation of photo-generated charge separation and charge injection to the maximum extent; (2) the GaN of the porous structure has the characteristic of adjustable band gap and can be matched with the perovskite and cathode structures better. Therefore, GaN material is a suitable choice as an electron transport layer of the light emitting diode, which can improve the quantum efficiency of the device.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a perovskite light emitting diode taking a GaN semiconductor material as an electron transport layer and a preparation method thereof. The perovskite light-emitting diode based on different types of GaN materials as an electron transport layer comprises a conductive glass layer (ITO), a hole transport layer, a perovskite layer, an electron transport layer and a metal counter electrode layer from bottom to top. The invention adopts a simple spin coating process, and takes the GaN semiconductor single crystal with a porous structure as the electron transmission layer of the perovskite light emitting diode, thereby increasing the contact area with the perovskite layer, slowing down the decomposition of the perovskite layer and improving the stability. Therefore, the invention adopts the following technical scheme:
a preparation method of a perovskite light emitting diode with GaN semiconductor material as an electron transport layer comprises the following steps:
(1) sputtering the compact nickel oxide film on the ITO conductive glass from the nickel oxide target material by a magnetron sputtering method;
(2) spin-coating CH on the NiO substrate in the step (1) by adopting a dip spin coating method3NH3PbBr3Or CH3NH3PbI3The perovskite precursor solution is quickly transferred to a preheated heating table after deposition is finished so that perovskite crystals are prepared into CH3NH3PbBr3、CH3NH3PbI3A perovskite light emitting layer;
(3) spin-coating the GaN suspension on the perovskite layer at the speed of 1500-3500r/min for 20-40s, standing for a period of time to volatilize the absolute ethyl alcohol, and completing the preparation of the electron transport layer;
(4) and (4) evaporating a gold electrode onto the electron transport layer prepared in the step (3) by using an electrode evaporation instrument, wherein the thickness of the gold electrode is 80nm, and obtaining the perovskite light-emitting diode with the GaN semiconductor material as the electron transport layer.
Preferably, in the step (2), CH is prepared in advance in a mixed solution of N, N-dimethyl imide (DMF, Sigma-Aldrich, 99.8%) and dimethyl sulfoxide (DMSO, Sigma-Aldrich, 99.8%)3NH3PbBr3And CH3NH3PbI3And (3) solution.
Preferably, the spin coating speed in the step (2) is 2000-5000r/min, the spin coating time is 40-80s, and the anti-solvent chlorobenzene is added dropwise at the time of 30-50 s.
Preferably, the temperature of the heating table in the step (2) is 80-120 ℃, and the heat preservation time is 40-80 min.
Preferably, the GaN electron transport layer in step (3) includes: GaN nano polycrystalline particles, GaN nano single crystal particles, two-dimensional GaN single crystal wafers and porous two-dimensional GaN single crystal wafers.
Preferably, the method for preparing a porous GaN suspension in step (3) includes the steps of: dissolving the GaN material in absolute ethyl alcohol, and then carrying out ultrasonic treatment to disperse the GaN material into GaN suspension.
Preferably, the spin coating speed in the step (3) is 2000r/min, and the spin coating time is 25 s.
Preferably, the electrode in the step (4) is gold, and the thickness of the electrode is 50-100 nm.
The invention also comprises a perovskite light emitting diode with the GaN semiconductor material obtained by the method as an electron transport layer.
Compared with the prior art, the invention has the following advantages:
the invention adopts a simple spin coating process, and takes the two-dimensional GaN material or GaN semiconductor material with a porous structure as the electron transmission layer of the perovskite light-emitting diode, thereby increasing the contact area with the perovskite layer, simultaneously slowing down the decomposition of the perovskite layer and improving the stability.
Drawings
FIG. 1 is a schematic structural view of a perovskite-type light emitting diode of the present invention;
FIG. 2 is an SEM scan of a two-dimensional GaN single crystal wafer;
FIG. 3 is CH3NH3PbBr3Infrared spectrogram after compounding with porous GaN;
FIG. 4 is CH3NH3PbBr3XPS full spectrum after compounding with porous GaN.
Detailed Description
The invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1: preparation method of perovskite light-emitting diode with GaN semiconductor material as electron transport layer
The method comprises the following steps:
(1) and (3) sequentially cleaning the ITO coated glass for 15min by using a detergent, acetone, isopropanol and deionized water, and then treating the ITO coated glass in ultraviolet ozone for 20 min.
(2) Sputtering the compact nickel oxide film on the ITO conductive glass from the nickel oxide target material by a magnetron sputtering method;
(3) in N2In a glove box, 100uL CH3NH3PbBr3The precursor solution is spin-coated on the NiO substrate for 45s at the speed of 4000rpm, and 200uL of anti-solvent chlorobenzene is quickly added at the 30 th s; then, the sample is kept warm for 15min on a heating table at 100 ℃ to ensure that the perovskite is crystallized to prepare CH3NH3PbBr3A perovskite light emitting layer;
preparing a perovskite precursor solution: 367mg of PbBr2And 112mg of methyl ammonium bromide (MABr) in 700uL of DMF and 78uL of DMSO, and stirring the mixture for 1 hour on a magnetic stirrer to prepare MAPbBr3A perovskite precursor solution. DMF: the volume ratio of DMSO is 9: 1.
(4) spin-coating 100uLGaN nano-polycrystalline dispersion onto the perovskite layer at 2000rpm for 20s, and then, allowing the sample to stand for a period of time to volatilize the absolute ethanol in the sample;
preparing GaN nano polycrystalline dispersion liquid: 1g of GaN nano-polycrystalline particles was dissolved in 1ml of absolute ethanol, and then subjected to ultrasonic treatment for 30min to disperse them.
(5) And (3) evaporating a gold electrode onto the prepared electron transport layer by an electrode evaporation instrument, wherein the thickness of the electrode is 80nm, and the preparation of the perovskite light-emitting diode with the GaN semiconductor material as the electron transport layer is completed.
Example 2: preparation method of perovskite light-emitting diode with GaN semiconductor material as electron transport layer
The method comprises the following steps:
(1) and (3) sequentially cleaning the ITO coated glass for 15min by using a detergent, acetone, isopropanol and deionized water, and then treating the ITO coated glass in ultraviolet ozone for 20 min.
(2) Sputtering the compact nickel oxide film on the ITO conductive glass from the nickel oxide target material by a magnetron sputtering method;
(3) in N2In a glove box, 100uL CH3NH3PbI3The precursor solution was spin coated onto the NiO substrate at 4000rpm for 45s, and 200uL of the anti-solvent chlorobenzene was added rapidly at 30 s. Then, the sample is kept warm for 15min on a heating table at 100 ℃ to ensure that the perovskite is crystallized to prepare CH3NH3PbI3A perovskite light emitting layer;
preparing a perovskite precursor solution: 460mg of PbI2And 159mg of Methyl Ammonium Iodide (MAI) were dissolved in 700uL of a mixed solution of DMF and 78uL of DMSO, and the solution was stirred for 1 hour on a magnetic stirrer to prepare MAPbI3A perovskite precursor solution. DMF: the volume ratio of DMSO is 9: 1.
(4) 100uL of GaN nano-single crystal dispersion was spin-coated on the perovskite layer at a speed of 2000rpm for 20s, and then the sample was left to stand for a period of time to volatilize the anhydrous ethanol in the sample.
Preparing GaN nano single crystal dispersion liquid: 1g of GaN nano single crystal particles was dissolved in 1ml of anhydrous ethanol, and then subjected to ultrasonic treatment for 30min to disperse them.
(5) And (3) evaporating a gold electrode onto the prepared electron transport layer by an electrode evaporation instrument, wherein the thickness of the electrode is 80nm, and the preparation of the perovskite light-emitting diode with the GaN semiconductor material as the electron transport layer is completed.
Example 3: preparation method of perovskite light-emitting diode with GaN semiconductor material as electron transport layer
The method comprises the following steps:
(1) and (3) sequentially cleaning the ITO coated glass for 15min by using a detergent, acetone, isopropanol and deionized water, and then treating the ITO coated glass in ultraviolet ozone for 20 min.
(2) Sputtering the compact nickel oxide film onto the ITO conductive glass from the nickel oxide target material by a magnetron sputtering method.
(3) In N2In a glove box, 100uL CH3NH3PbI3The precursor solution was spin coated onto the NiO substrate 45s at 4000rpm, and 200uL of the anti-solvent chlorobenzene was added rapidly at 30 s. Then, the sample is kept warm for 15min on a heating table at 100 ℃ to ensure that the perovskite is crystallized to prepare CH3NH3PbI3A perovskite light emitting layer;
preparing a perovskite precursor solution: 460mg of PbI2And 159mg of Methyl Ammonium Iodide (MAI) were dissolved in 700uL of a mixed solution of DMF and 78uL of DMSO, and the solution was stirred for 1 hour on a magnetic stirrer to prepare MAPbI3A perovskite precursor solution. DMF: the volume ratio of DMSO is 9: 1.
(4) 100uL of the two-dimensional GaN single-wafer dispersion was spin-coated on the perovskite layer at a speed of 2000rpm for 20 seconds, and then the sample was left to stand for a period of time to volatilize the absolute ethanol in the sample.
Preparing two-dimensional GaN single-chip dispersion liquid: 1g of a two-dimensional GaN single crystal wafer was dissolved in 1ml of anhydrous ethanol, and then subjected to ultrasonic treatment for 30min to disperse it.
(5) And (3) evaporating a gold electrode onto the prepared electron transport layer by an electrode evaporation instrument, wherein the thickness of the electrode is 80nm, and the preparation of the perovskite light-emitting diode with the GaN semiconductor material as the electron transport layer is completed.
Example 4: preparation method of perovskite light-emitting diode with GaN semiconductor material as electron transport layer
The method comprises the following steps:
(1) and (3) sequentially cleaning the ITO coated glass for 15min by using a detergent, acetone, isopropanol and deionized water, and then treating the ITO coated glass in ultraviolet ozone for 20 min.
(2) Sputtering the compact nickel oxide film onto the ITO conductive glass from the nickel oxide target material by a magnetron sputtering method.
(3) In N2In a glove box, 100uL CH3NH3PbBr3The precursor solution was spin coated onto the NiO substrate at 4000rpm for 45s, and 200uL of the anti-solvent chlorobenzene was added rapidly at 30 s. Then, the sample is kept warm for 15min on a heating table at 100 ℃ to ensure that the perovskite is crystallized to prepare CH3NH3PbBr3A perovskite light emitting layer;
preparing a perovskite precursor solution: 367mg of PbBr2And 112mg of methyl ammonium bromide (MABr) in 700uL of DMF and 78uL of DMSO, and stirring the mixture for 1 hour on a magnetic stirrer to prepare MAPbBr3A perovskite precursor solution. DMF: the volume ratio of DMSO is 9: 1.
(4) 100uL of the porous two-dimensional GaN single crystal dispersion was spin-coated on the perovskite layer at a speed of 2000rpm for 20s, and then the sample was left to stand for a period of time to volatilize the anhydrous ethanol in the sample.
Preparation of porous two-dimensional GaN single crystal dispersion: 1g of the porous two-dimensional GaN single crystal wafer was dissolved in 1ml of anhydrous ethanol, and then subjected to ultrasonic treatment for 30min to disperse it.
(5) And (3) evaporating a gold electrode onto the prepared electron transport layer by an electrode evaporation instrument, wherein the thickness of the electrode is 80nm, and the preparation of the perovskite light-emitting diode with the GaN semiconductor material as the electron transport layer is completed.
Test example:
through detection: an SEM scanning image of the two-dimensional GaN single crystal wafer is shown in FIG. 2; CH (CH)3NH3PbBr3The infrared spectrogram after the composition with the porous GaN is shown in FIG. 3; CH (CH)3NH3PbBr3The XPS survey spectrum after recombination with porous GaN is shown in FIG. 4.
Claims (8)
1. A preparation method of a perovskite light emitting diode with a GaN semiconductor material as an electron transport layer is characterized by comprising the following steps:
(1) sputtering the compact nickel oxide film on the ITO conductive glass from the nickel oxide target material by a magnetron sputtering method;
(2) spin-coating CH on the NiO substrate in the step (1) by adopting a dip spin coating method3NH3Br or CH3NH3I perovskite precursor solution is quickly transferred to a preheated heating table after deposition is finished so as to crystallize perovskite to prepare CH3NH3Br、CH3NH3I perovskite light emitting layer;
(3) spin-coating the GaN suspension on the perovskite layer at the speed of 1500-3500r/min for 20-40s, standing for a period of time to volatilize the absolute ethyl alcohol, and completing the preparation of the electron transport layer;
(4) and (4) evaporating a gold electrode onto the electron transport layer prepared in the step (3) by using an electrode evaporation instrument, wherein the thickness of the gold electrode is 80nm, and obtaining the perovskite light-emitting diode with the GaN semiconductor material as the electron transport layer.
2. The method according to claim 1, wherein the CH is prepared in advance in the mixed solution of N, N-dimethyl imide and dimethyl sulfoxide in the step (2)3NH3PbBr3And CH3NH3PbI3And (3) solution.
3. The preparation method as claimed in claim 1, wherein the spin coating speed in step (2) is 2000-5000r/min, the spin coating time is 40-80s, and the anti-solvent chlorobenzene is added at 30-50 s.
4. The method according to claim 1, wherein the heating stage temperature in the step (2) is 80-120 ℃ and the holding time is 40-80 min.
5. The production method according to claim 1, wherein the GaN electron transport layer in the step (3) comprises: at least one of GaN nano polycrystalline particles, GaN nano single crystal particles, two-dimensional GaN single crystal wafers and porous two-dimensional GaN single crystal wafers.
6. The method according to claim 1, wherein the GaN suspension in step (3) is prepared by: dissolving the GaN material in absolute ethyl alcohol, and then carrying out ultrasonic treatment to disperse the GaN material into GaN suspension.
7. The production method according to claim 1, wherein the spin coating speed in the step (3) is 2000r/min and the spin coating time is 25 s.
8. A perovskite light emitting diode having a GaN semiconductor material obtained by the production method as defined in any of claims 1 to 7 as an electron transport layer.
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