CN114920282A - Perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof - Google Patents

Perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof Download PDF

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CN114920282A
CN114920282A CN202210758099.6A CN202210758099A CN114920282A CN 114920282 A CN114920282 A CN 114920282A CN 202210758099 A CN202210758099 A CN 202210758099A CN 114920282 A CN114920282 A CN 114920282A
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perovskite
precursor solution
substrate
gan
solution
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俞娇仙
李秋波
张雷
刘光霞
陈成敏
王国栋
王守志
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Qilu University of Technology
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Abstract

A perovskite nanocrystalline growing on a GaN monocrystal substrate and a preparation method thereof are disclosed, the preparation method comprises the following steps: (1) sequentially cleaning the GaN single crystal substrate by using acetone, isopropanol and deionized water, and then treating in an ultraviolet plasma cleaning instrument; (2) preparing a perovskite precursor solution; (3) preparing perovskite nanocrystal: spin-coating the perovskite precursor solution on a GaN substrate, and adding an anti-solvent chlorobenzene in the spin-coating process; and standing after the spin coating is finished, and then placing on a heating table for heat preservation to enable perovskite crystals to be prepared into the halogen perovskite nanocrystals. The method has the advantages of simple and convenient operation, low cost and easy large-area film formation, and the obtained perovskite nanocrystal has the characteristics of good uniformity, high crystallization quality, wide visible light absorption range and the like.

Description

Perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof
Technical Field
The invention relates to a perovskite nanocrystal grown on a GaN monocrystal substrate and a preparation method thereof, belonging to the technical field of perovskite nanomaterials.
Background
Halide perovskite AMX 3 (wherein A ═ CH) 3 NH 3 + ，CH(NH 2 ) 2 + ，Cs + ；M＝Pb 2+ ，Sn 2+ ；X＝I - ，Br - ，Cl - ) Nanocrystalline thin films have become a promising next generation of luminescent materials due to their spectral tunability, narrow emission, high quantum efficiency, and solution processibility. These characteristics may enable the use of perovskite light sources with a wide color reproduction range, excellent color purity, high brightness, and low power consumption. In many halide perovskites, the binding energy of the exciton is sufficiently low to spontaneously dissociate into free electrons and holes at room temperature. This reduces the rate of radiative recombination, allows competition for non-radiative assisted recombination at defect sites, and reduces the quantum efficiency achievable at low carrier densities. However, halide perovskites tend to be unstable to ambient air and humidity, which instability may cause abnormal operation of the device at bias voltages.
Encapsulation in an impermeable matrix of a more stable material is one strategy to protect the perovskite from environmental degradation. It is reported that GaN/AMX is formed when GaN single crystal wafer is used as substrate for growing halide perovskite 3 The system also forms an I-type heterojunction, the band gap of GaN spans the band gap of perovskite, and the carrier confinement can be enhanced by inhibiting the carrier wave work leakage of perovskite. Experiments have shown that environmental degradation of GaN-coated perovskites is significantly slowed, even in ambient atmosphereThe green photoluminescence characteristic of the perovskite can be still preserved for 1 year. The blue shift of the emission peak wavelength and the emission intensity also show a proportional correlation trend. From a crystal growth perspective, the atomically smooth surface of the GaN wafer has a large number of atomically sharp dangling bonds and dislocations, providing sites for uniform nucleation and heteroepitaxial deposition of perovskites. At present, two film forming modes of perovskite nanocrystalline mainly comprise evaporation and spin coating, but the evaporation method needs high vacuum environment, high evaporation temperature and other preparation conditions, and is not beneficial to large-scale production of films.
Disclosure of Invention
The invention provides a perovskite nanocrystalline growing on a GaN monocrystal substrate and a preparation method thereof, the preparation method has the advantages of simple and convenient operation, low cost and easy large-area film formation, and the perovskite nanocrystalline obtained by the method has the characteristics of good uniformity, high crystallization quality, wide visible light absorption range and the like from a scanning electron microscope and visible light absorption spectrum tests.
A preparation method for growing perovskite nanocrystalline on a GaN single crystal substrate comprises the following steps:
(1) sequentially cleaning the GaN single crystal substrate by using acetone, isopropanol and deionized water, and then treating in an ultraviolet plasma cleaning instrument;
(2) preparing a perovskite precursor solution:
mixing DMF and DMSO at room temperature according to the volume ratio of 9:1 to obtain a mixed solution A for later use;
② weighing analytically pure methyl amine halide (MAX) or cesium halide (CsX), and then mixing with lead halide PbY 2 Adding the powder into the mixture A, wherein MAX or CsX and PbY are respectively 2 The mass ratio of the powder is 1: 1; then placing the perovskite precursor solution on a magnetic stirrer, stirring the perovskite precursor solution until the perovskite precursor solution is completely dissolved, and filtering the solution to obtain a clear solution to obtain a perovskite precursor solution;
(3) preparing perovskite nanocrystalline: spin-coating the perovskite precursor solution on a GaN substrate at the speed of 3000-5000rpm for 45s, and rapidly adding an anti-solvent chlorobenzene when the spin-coating time reaches 30 s; standing for 3-5min after the spin coating is finished, and then placing on a heating table with the temperature of 100-220 ℃ for heat preservation for 15min to enable the perovskite crystal to prepare the halogen perovskite nanocrystalline.
According to the present invention, preferably, the GaN single crystal substrate used in the step (1) is an n-type GaN single crystal substrate grown on a double-side polished sapphire substrate by a Metal Organic Chemical Vapor Deposition (MOCVD).
According to the invention, in the step (1), the GaN single crystal substrate is sequentially cleaned by acetone, isopropanol and deionized water for 15min, and then treated in an ultraviolet plasma cleaning instrument for 20 min.
According to the invention, the stirring time of the organic-inorganic hybrid perovskite precursor solution in the step (2) is preferably 1h, and the all-inorganic hybrid perovskite precursor solution is magnetically stirred for 24h under the condition of a water bath with the constant temperature of 60 ℃.
Preferably, in the step (2), the MAX is at least one of methylammonium chloride (MACl), methylammonium bromide (MABr) and methylammonium iodide (MAI), CsX is at least one of cesium chloride (CsCl), cesium bromide (CsBr) and cesium iodide (CsI), and the PbY is 2 Is PbCl 2 、PbBr 2 And PbI 2 At least one of (a).
According to the invention, the substrate selected in the step (3) is preferably a GaN substrate.
According to the invention, the spin-coating speed in the step (3) is 4000r/min, and the spin-coating time of the anti-solvent chlorobenzene is not higher than 15 s.
According to the invention, preferably, the perovskite solution in the step (3) needs to be kept for 5min after the spin coating.
According to the invention, in the step (3), the annealing temperature after the spin coating of the organic-inorganic hybrid perovskite solution is 100 ℃, and the annealing temperature after the spin coating of the all-inorganic hybrid perovskite solution is 220 ℃.
The invention also discloses the perovskite nanocrystal obtained by the preparation method.
Compared with the prior art, the invention has the following advantages:
x in perovskite precursor solution - And Y - The proportion of the components can be determined according to the required purposePreparing the target product by controlling I in the perovskite precursor solution - 、Cl - 、Br - The concentration of the perovskite nano-crystalline can adjust the emission wavelength of the product nano-crystalline, so that the perovskite nano-crystalline material which can emit light in the full wave band within the visible light range can be prepared.
From the perspective of crystal growth, the GaN single crystal wafer is selected as the substrate, and the GaN wafer has the advantages that the smooth atomic surface has a large number of sharp dangling bonds and dislocations on atoms, and sites are provided for uniform nucleation and heteroepitaxial deposition of perovskite.
Drawings
FIG. 1 shows MAPbBr 3 Scanning electron microscopy images of perovskite nanocrystals;
FIG. 2 shows MAPbBr 3 An XRD spectrum of the perovskite nanocrystal;
FIG. 3 shows MAPbBr 3 A visible light absorption spectrum of the perovskite nanocrystal;
FIG. 4 shows MAPbBr 3 PL spectrum of perovskite nanocrystals.
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 substitutions are intended to be within the scope of the invention.
Example 1: perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof
(1) And (3) sequentially cleaning the n-type GaN single crystal substrate growing on the double-sided polished sapphire substrate by the MOCVD method for 15min by using acetone, isopropanol and deionized water, and then treating for 20min in an ultraviolet plasma cleaning instrument.
(2) Preparing a perovskite precursor solution: taking 700uL of DMF and 78uL of DMSO, and enabling the volume ratio of the two reagents to be 9:1, mixing DMF and DMSO at room temperature for later use.
(3) According to the following steps: 1 the purity is weighed as analytical purityMABr and PbBr of 2 And adding 0.1mol of powder into the mixed solution respectively, then placing the mixed solution on a magnetic stirrer to stir for 1 hour, and filtering to obtain a clear solution, namely the precursor solution required by the preparation of the perovskite nanocrystal.
(4) Preparing perovskite nanocrystalline: 100uL of MAPbBr 3 Spin-coating the precursor solution on a GaN substrate at the speed of 4000rpm for 45s, and rapidly adding 200uL of anti-solvent chlorobenzene when the spin-coating time reaches 30 s; standing for 5min after the spin coating is finished, and then placing on a heating table at 100 ℃ for heat preservation for 15min to make perovskite crystal into MAPbBr 3 Perovskite nanocrystals.
FIG. 1 shows the MAPbBr prepared in this example 3 Perovskite nanocrystals, it can be seen that the size of the nanocrystals is relatively uniform. FIG. 2 shows MAPbBr 3 The XRD pattern of the perovskite nanocrystal proves that the component is MAPbBr 3 . FIG. 3 shows MAPbBr 3 The visible light absorption spectrum of the perovskite nanocrystalline relates to the whole visible light region. FIG. 4 shows MAPbBr 3 PL map of perovskite nanocrystal shows GaN and MAPbBr 3 Characteristic peak of (2).
Example 2: perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof
(1) And (3) sequentially cleaning the n-type GaN single crystal substrate growing on the double-sided polished sapphire substrate by the MOCVD method for 15min by using acetone, isopropanol and deionized water, and then treating for 20min in an ultraviolet plasma cleaning instrument.
(2) Preparing a perovskite precursor solution: taking 700uL of DMF and 78uL of DMSO, wherein the volume ratio of the two reagents is 9:1, mixing DMF and DMSO at room temperature for later use.
(3) According to the following steps: 1 CsBr and PbBr of analytically pure purity were weighed 2 Adding 0.1mol of each powder into the mixed solution, and then placing the mixed solution under the condition of water bath at the constant temperature of 60 ℃ for magnetic stirring for 24 hours to completely dissolve; filtering to obtain a clear solution, namely the precursor solution required by the preparation of the perovskite nanocrystalline.
(4) Preparing perovskite nanocrystal: mixing 100uL CsPbBr 3 The precursor solution is spin-coated on the GaN substrate at the speed of 4000rpm for 45s, and spin-coating is carried outAdding 200uL of anti-solvent chlorobenzene quickly when 30s is reached; standing for 5min after the spin coating is finished, and then placing on a heating table at 100 ℃ for heat preservation for 15min to make the perovskite crystallized to obtain CsPbBr 3 A perovskite nanocrystal.
Example 3: perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof
(1) And (3) sequentially cleaning the n-type GaN single crystal substrate grown on the double-sided polished sapphire substrate by using an MOCVD method for 15min by using acetone, isopropanol and deionized water, and then treating for 20min in an ultraviolet plasma cleaning instrument.
(2) Preparing a perovskite precursor solution: taking 700uL of DMF and 78uL of DMSO, wherein the volume ratio of the two reagents is 9: DMF and DMSO are mixed at room temperature for later use.
(3) According to the proportion of 1:1, weighing MAI and PbI with purities of analytical purity 2 And adding 0.1mol of powder into the mixed solution respectively, then placing the mixed solution on a magnetic stirrer, stirring the mixed solution for 1 hour, and filtering the mixed solution to obtain a clear solution, namely the precursor solution required by the preparation of the perovskite nanocrystal.
(4) Preparing perovskite nanocrystalline: 100uL MAPbI 3 The precursor solution is spin-coated on a GaN substrate at the speed of 4000rpm for 45s, and 200uL of anti-solvent chlorobenzene is rapidly added when the spin-coating time reaches 30 s; standing for 5min, and keeping at 100 deg.C for 15min to obtain MAPbI 3 Perovskite nanocrystals.
Example 4: perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof
(1) And (3) sequentially cleaning the n-type GaN single crystal substrate growing on the double-sided polished sapphire substrate by the MOCVD method for 15min by using acetone, isopropanol and deionized water, and then treating for 20min in an ultraviolet plasma cleaning instrument.
(2) Preparing a perovskite precursor solution: taking 700uL of DMF and 78uL of DMSO, wherein the volume ratio of the two reagents is 9:1, mixing DMF and DMSO at room temperature for later use.
(3) According to the proportion of 1:1 weighing CsI and PbI with purity of analytical purity 2 Adding 0.1mol of the powder into the above mixed solution, and placing in a water bath bar at constant temperature of 60 deg.CStirring for 24h under magnetic force to completely dissolve; filtering to obtain a clear solution, namely the precursor solution required by the preparation of the perovskite nanocrystalline.
(4) Preparing perovskite nanocrystalline: mixing 100uL CsPbI 3 Spin-coating the precursor solution on a GaN substrate at the speed of 4000rpm for 45s, and rapidly adding 200uL of anti-solvent chlorobenzene when the spin-coating time reaches 30 s; standing for 5min after spin coating, and keeping the temperature on a heating table at 100 deg.C for 15min to obtain CsPbI 3 Perovskite nanocrystals.

Claims (10)

1. A preparation method for growing perovskite nanocrystalline on a GaN single crystal substrate is characterized by comprising the following steps:
(1) sequentially cleaning the GaN single crystal substrate by using acetone, isopropanol and deionized water, and then treating in an ultraviolet plasma cleaning instrument;
(2) preparing a perovskite precursor solution:
mixing DMF and DMSO at room temperature according to the volume ratio of 9:1 to obtain a mixed solution A for later use;
② weighing analytically pure methyl amine halide (MAX) or cesium halide (CsX), and then mixing with lead halide PbY 2 Adding the powder into the mixture A, wherein MAX or CsX, and PbY 2 The mass ratio of the powder is 1: 1; then placing the perovskite precursor solution on a magnetic stirrer, stirring the perovskite precursor solution until the perovskite precursor solution is completely dissolved, and filtering the solution to obtain a clear solution to obtain a perovskite precursor solution;
(3) preparing perovskite nanocrystal: spin-coating the perovskite precursor solution on a GaN substrate at the speed of 3000-; standing for 3-5min after the spin coating is finished, and then placing on a heating table with the temperature of 100-220 ℃ for heat preservation for 15min to enable the perovskite crystal to prepare the halogen perovskite nanocrystalline.
2. The production method according to claim 1, wherein the GaN single-crystal substrate used in the step (1) is an n-type GaN single-crystal substrate grown on a double-side polished sapphire substrate by a metal organic chemical vapor deposition method.
3. The method according to claim 1, wherein in step (1), the GaN single crystal substrate is sequentially cleaned with acetone, isopropanol and deionized water for 15min and then treated in an ultraviolet plasma cleaner for 20 min.
4. The preparation method according to claim 1, wherein the stirring time of the organic-inorganic hybrid perovskite precursor solution in the step (2) is 1h, and the all-inorganic hybrid perovskite precursor solution is magnetically stirred for 24h under the condition of a water bath with a constant temperature of 60 ℃.
5. The method of claim 1, wherein in step (2), the MAX is at least one of methylammonium chloride (MACl), methylammonium bromide (MABr) and methylammonium iodide (MAI), CsX is at least one of cesium chloride (CsCl), cesium bromide (CsBr) and cesium iodide (CsI), and PbY 2 Is PbCl 2 、PbBr 2 And PbI 2 At least one of (1).
6. The production method according to claim 1, wherein the substrate selected in the step (3) is a GaN substrate.
7. The method according to claim 1, wherein the spin coating speed in step (3) is 4000r/min, and the spin coating time of the anti-solvent chlorobenzene is not higher than 15 s.
8. The production method according to claim 1, wherein the perovskite solution in the step (3) is allowed to stand for 5min after the spin coating.
9. The preparation method according to claim 1, wherein the annealing temperature after the spin coating of the organic-inorganic hybrid perovskite solution in the step (3) is 100 ℃ and the annealing temperature after the spin coating of the all-inorganic hybrid perovskite solution is 220 ℃.
10. Perovskite nanocrystals obtainable by the production process as claimed in any one of claims 1 to 9.
CN202210758099.6A 2022-06-30 2022-06-30 Perovskite nanocrystalline growing on GaN monocrystal substrate and preparation method thereof Pending CN114920282A (en)

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Application publication date: 20220819