CN114163991A - Perovskite nanocrystalline with stable appearance at high temperature and preparation method thereof - Google Patents
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Abstract
The invention discloses a perovskite nanocrystalline with stable appearance at high temperature and a preparation method thereof. The method comprises the following specific steps: a. mixing Cs (CH)3Mixing COOH), octadecene and oleic acid, and carrying out heating reaction under the condition of protective atmosphere to obtain a cesium oleate precursor solution; b. dissolving lead halide in a mixture of octadecene, oleic acid and oleylamine under a protective atmosphere at a high temperature; c. dissolving halide doped with metal in a mixture of octadecene, oleic acid and oleylamine at high temperature under a protective atmosphere to obtain transparent liquid. d. Subjecting the mixture obtained in step a toAnd (e) rapidly injecting a cesium precursor into the liquid in the step (b), reacting for 1 minute, then injecting the transparent liquid in the step (c), reacting for 30 minutes, rapidly cooling to room temperature, and e, centrifugally purifying to obtain the doped perovskite nanocrystal with stable morphology at high temperature.
Description
Technical Field
The invention belongs to the field of nanocrystalline materials, and particularly relates to a perovskite nanocrystalline with stable appearance at high temperature and a preparation method thereof.
Background
The all-inorganic perovskite nanocrystal is an excellent luminescent material, but the all-inorganic perovskite nanocrystal is easy to lose surface ligands at high temperature and cause agglomeration and growth. This not only severely limits the application of perovskite nanocrystals to high-energy LEDs, lasers and solar cells but also hinders surface engineering of perovskite nanocrystals.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for obtaining a perovskite nanocrystal with stable morphology at high temperature, and the perovskite nanocrystal obtained by the present invention has good morphology stability at high temperature.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the perovskite nanocrystal with stable appearance at high temperature comprises the following steps:
(1) mixing Cs (CH3COOH), octadecene and oleic acid, heating for 20-60min at 160 ℃ under the protective atmosphere of 140-;
(2) dissolving lead halide in a mixture of octadecene, oleic acid and oleylamine at 180-200 ℃ under a protective atmosphere to obtain a lead precursor solution, and keeping the lead precursor solution at 180-200 ℃ for later use;
(3) dissolving doped metal halide in a mixture of octadecene, oleic acid and oleylamine at a high temperature of 150-180 ℃ under a protective atmosphere for reacting for 20-60min to obtain a transparent doped metal precursor solution, and keeping the temperature at 80-130 ℃ for later use;
(4) injecting the cesium precursor solution in the step (1) into the lead precursor solution in the step (2), reacting for 1-5min to obtain a perovskite nanocrystalline mother solution, injecting the doped metal precursor solution in the step (3) into the perovskite nanocrystalline mother solution, and reacting for 5-180 min to obtain a nanocrystalline solution;
(5) and (4) carrying out centrifugal purification on the nanocrystalline solution obtained in the step (4) under the condition of 3000 r/min, and dissolving the nanocrystalline precipitate in a nonpolar solvent to obtain the perovskite nanocrystalline with stable appearance at high temperature.
Further, Cs (CH) in the step (1)3COOH) and oleic acid at a molar ratio of 1: 1.5-1: 3; the Cs (CH)3COOH) in octadecene and oleic acid at a molar concentration of 0.05-0.15 mmol/ml.
Further, the molar ratio of the lead halide to the oleic acid in the step (2) is 1: 1-1: and 2, the molar ratio of the oleic acid to the oleylamine is 1: 0.75-1: 1.5, the molar concentration of the lead halide in the mixture of octadecene, oleic acid and oleylamine is 0.05-0.15 mmol/ml.
Further, the molar ratio of the doped metal halide to the oleic acid in the step (3) is 1: 1-1: 2; the mol ratio of oleic acid to oleylamine was 1: 0.8-1: 1.2, the molar concentration of the metal-doped halide in the mixture of octadecene, oleic acid and oleylamine is 0.2-0.8 mmol/ml.
Further, the metal halide doped in the step (3) is ZnX2、MgX2、CaX2Or MnX2Wherein X = Cl, Br or I.
Further, the reaction temperature in the step (4) is 180-200 ℃.
Further, the molar ratio of the doping metal in the doping metal precursor solution in the step (4) to the lead ions in the perovskite nanocrystalline mother solution is 1: 0.5-1: 5.
the surface chemistry of the perovskite nanocrystal is regulated and controlled by means of metal ion doping, the bonding of the nanocrystal and the ligand is enhanced, and the ligand is inhibited from being separated at high temperature, so that the high-temperature stability of the perovskite nanocrystal is improved. The method provided by the invention can obtain the perovskite nanocrystalline which is stable at high temperature (more than 180 ℃), and the obtained perovskite nanocrystalline has good monodispersity, good monochromaticity and half-peak width smaller than 20 nanometers, thereby providing an important basis for further carrying out structural control on the nanocrystalline.
Drawings
FIG. 1 is a graph of the original perovskite nanocrystal obtained in example 1 under high temperature evolution;
FIG. 2 is a transmission electron microscope image of the zinc-doped perovskite nanocrystal obtained in example 2 after heating at a high temperature of 200 ℃ for different times;
FIG. 3 is a transmission electron microscope image of the manganese-doped perovskite nanocrystal obtained in example 3 after heating at a high temperature of 200 ℃ for different times.
Detailed Description
The invention provides a synthesis method of a high-temperature stable perovskite nanocrystal, which comprises the following steps:
a. mixing Cs (CH)3Mixing COOH), octadecene and oleic acid, heating to 150 ℃ in a nitrogen atmosphere, reacting for 30 minutes to obtain a cesium precursor, and keeping the temperature at 150 ℃ for later use;
b. dissolving lead halide in a mixture of octadecene, oleic acid and oleylamine at 180-200 ℃ under the protection of nitrogen to obtain a lead precursor, and keeping the lead precursor at 180-200 ℃ for later use;
c. dissolving metal-doped halide in octadecene, oleic acid and oleylamine at a high temperature of 150-170 ℃ in a nitrogen protective manner to obtain a transparent metal-doped precursor solution, and keeping the temperature at 100 ℃ for later use;
d. injecting the cesium precursor obtained in the step a into the lead precursor obtained in the step b, reacting for 1 minute, injecting the doped metal halide precursor obtained in the step c, and reacting for 5-180 minutes;
e. and d, carrying out centrifugal purification on the quantum dot solution obtained in the step d for 5 minutes under the condition of 3000 r/min, and dissolving the quantum dot precipitate in toluene to obtain the perovskite quantum dot solution.
Specifically, the present invention relates to Cs (CH)3COOH), octadecene and oleic acid. Wherein Cs (CH)3COOH) to oleic acid molar ratio of 1: 1.5-1: 3, preferably 1: 2.5. the Cs (CH)3COOH) in a mixture of octadecene and oleic acid in a molar concentration of 0.05-0.15 mmol/ml, preferably 0.07 mol/L.
Then, the mixture was heated to react under nitrogen protection. Wherein the heating reaction temperature is 140-160 ℃, and preferably 150-157 ℃. The reaction time is 20 to 60 minutes, preferably 30 to 40 minutes. After the reaction is finished, the obtained transparent solution is kept at the temperature of 120-160 ℃, and preferably 140-155 ℃.
Then mixing lead halide with octadecene, oleic acid and oleylamine to obtain a mixture. The mixture was heated to react under a nitrogen atmosphere. The heating temperature is 160-200 ℃, preferably 180-200 ℃. The reaction time is 10 to 20 minutes, preferably 15 to 20 minutes. And after the reaction is finished, keeping the temperature of the obtained lead precursor transparent solution at 180-200 ℃ for later use. The lead halide is lead chloride, lead bromide or lead iodide.
The molar ratio of the lead halide to the oleic acid is 1: 1-1: 2, preferably 1: 1-1: 1.75. the molar ratio of oleic acid to oleylamine was 1: 0.75-1: 1.5, preferably 1: 0.8-1: 1.2. the molar concentration of the lead halide in the octadecene, oleic acid and oleylamine solution is 0.015-0.05 mmol/ml, and preferably 0.02-0.04 mmol/ml.
And heating the doped metal halide, octadecene, oleic acid and oleylamine for reaction. Wherein, the doped metal halide refers to ZnX2，MgX2，CaX2，MnX2(X = Cl, Br, I). The heating reaction temperature is 150-180 ℃, and preferably 160-180 ℃. The reaction time is 20 to 60 minutes, preferably 30 to 40 minutes. The molar ratio of the doped metal ions to the oleic acid is 1: 1-1: 2, preferably 1: 1.5-1: 1.75, the molar ratio of oleic acid to oleylamine is 1: 0.75-1: 1.5, preferably 1: 0.8-1: 1.2, the molar concentration of the doping metal in the octadecene, oleic acid and oleylamine solution is 0.2-0.8 mmol/mL, preferably 0.35-0.5 mmol/mL. After the reaction is finished, the obtained doped metal precursor is kept at 80-130 ℃, and preferably 100-120 ℃.
And injecting the cesium precursor into the lead precursor solution, and reacting for 1-5 minutes, preferably 1-2 minutes to obtain the perovskite nanocrystalline mother solution. The volume ratio of the cesium precursor to the lead precursor is 1: 10-1: 15, preferably 1: 11-1: 12.5.
and then injecting the doped metal precursor into the perovskite nanocrystalline mother solution, and heating for reaction to obtain a perovskite quantum dot doped crude solution. The reaction temperature is 180-200 ℃, preferably 185-195 ℃. The reaction time is 5-180 minutes, preferably 30-60 minutes, and the molar ratio of the doped metal in the doped metal precursor solution to the lead ions in the perovskite nanocrystalline mother solution is 1: 0.5-1: 5, preferably 1: 2-1: 4.
and carrying out centrifugal purification on the obtained perovskite quantum dot doped crude solution, collecting the lower-layer precipitate, and dissolving the precipitate in a non-polar organic solvent. The centrifugal speed is 3000 r/min, and the nonpolar organic solvent is hexane, octane, toluene, octadecene. After purification, the obtained perovskite nanocrystalline can keep stable in shape in octadecylene solvent at high temperature of 180-200 ℃.
The doped perovskite nanocrystalline with stable appearance at high temperature is synthesized by metal doping. By utilizing the strong interaction between the doped metal ions and the surface ligands, the desorption of the surface ligands can be effectively relieved, and the agglomeration growth of the nanocrystalline is inhibited. The method provides an important foundation for further improving the structural stability of the perovskite nanocrystal and promoting the application of the perovskite nanocrystal in the fields of high-energy LEDs, lasers, solar cells and the like.
For further understanding of the present invention, the following examples are provided to illustrate the preparation method of doped perovskite nanocrystals of the present invention, and the scope of the present invention is not limited by the following examples.
Example 1
This example is mainly demonstrated by the morphological instability of the metal ion doped perovskite nanocrystals of the present invention at high temperatures.
1. Weighing Cs (CH)3COOH) powder 0.12 g, oleic acid 0.3 ml, octadecene 5ml were charged into a 25ml three-necked flask. Wherein Cs (CH)3COOH) and oleic acid in a molar ratio of 1: 1.5, the molar concentration of cesium ions is 0.12 mmol/ml. And introducing nitrogen while magnetically stirring, deoxidizing for 30 minutes, heating the flask to 150 ℃, keeping for 30 minutes to obtain a light yellow transparent cesium precursor solution, and keeping the temperature at 150 ℃ for later use.
2. Weighing PbCl20.069 g of powder, 0.011g of ZnCl2 powder, 0.5 ml of oleic acid, 0.5 ml of oleylamine and 5ml of octadecene were put into a 25ml three-necked flask. Wherein PbCl2And oleic acid in a 1: 1, the molar ratio of oleic acid to oleylamine is 1.08: 1. the molar concentration of lead ions was 0.4 mmol/ml. Introducing nitrogen while magnetically stirring, removing oxygen for 30 min, heating to 195 deg.C, maintaining for 20 min to obtain yellowish transparent lead precursor solution, and adding 0.4 ml of cesiumAnd (3) rapidly adding the precursor solution, and rapidly cooling the reaction to room temperature after reacting for 1 minute to obtain a crude perovskite nanocrystal solution.
3. And (3) carrying out centrifugal purification on the obtained perovskite nanocrystalline crude solution for 5 minutes, wherein the centrifugal rotating speed is 3000 r/min. And dissolving the collected nano-crystals in octadecene to obtain a perovskite nano-crystal solution.
4. After heating the perovskite nanocrystalline solution to 180 ℃, sampling and observing the evolution of the morphology at high temperature in 1 minute, 30 minutes, 80 minutes and 120 minutes respectively. The results are shown in FIG. 1. It can be seen that the undoped perovskite nanocrystal loses the initial morphology thereof quickly at high temperature, and the agglomeration grows up.
Example 2
This example demonstrates that doped perovskite nanocrystals prepared according to the method of the present invention have good morphological stability at high temperatures.
1. Weighing Cs (CH)3COOH) powder 0.12 g, oleic acid 0.3 ml, octadecene 5ml were charged into a 25ml three-necked flask. Wherein Cs (CH)3COOH) and oleic acid in a molar ratio of 1: 1.5, the molar concentration of cesium ions is 0.12 mmol/ml. And introducing nitrogen while magnetically stirring, deoxidizing for 30 minutes, heating the flask to 150 ℃, keeping for 30 minutes to obtain a light yellow transparent cesium precursor solution, and keeping the temperature at 150 ℃ for later use.
2. Weighing PbCl20.069 g of powder, 0.5 ml of oleic acid, 0.5 ml of oleylamine and 5ml of octadecene were charged into a 25ml three-necked flask. Wherein PbCl2And oleic acid in a 1: 1, the molar ratio of oleic acid to oleylamine is 1.08: 1. the molar concentration of lead ions was 0.4 mmol/ml. Introducing nitrogen while magnetically stirring, deoxidizing for 30 min, heating to 195 deg.C, holding for 20 min to obtain yellowish transparent lead precursor solution, and holding the system at 195 deg.C
3. 0.136 g of ZnCl was weighed2Mixed with 5ml octadecene, 0.5 ml oleic acid and 0.5 ml oleylamine and charged into a 25ml three-necked flask. Wherein, ZnCl2The molar ratio to oleic acid was 1: 1.5, the molar ratio of oleic acid to oleylamine is 1.08: 1, the molar concentration of zinc ions is 0.17 mmol/ml. Introducing nitrogen under magnetic stirring, deoxidizing for 30 min, heating to 150 deg.C, and maintainingAnd (3) cooling the system to 100 ℃ after the temperature is 30 minutes to obtain a light yellow transparent zinc precursor solution for later use.
4. And then, quickly adding 0.4 ml of cesium precursor solution into lead precursor solution, reacting for 1 minute to obtain perovskite nanocrystalline mother solution, then adding 0.5 ml of zinc precursor solution, reacting for 30 minutes, and quickly cooling the reaction to room temperature to obtain crude solution doped with perovskite nanocrystalline.
5. And (3) carrying out centrifugal purification on the obtained perovskite nanocrystalline crude solution for 5 minutes, wherein the centrifugal rotating speed is 3000 r/min. And dissolving the collected nano-crystals in octadecene to obtain a perovskite nano-crystal solution.
6. After heating the doped perovskite nanocrystalline solution to 180 ℃, sampling and observing the evolution of the morphology at high temperature in 1 minute, 60 minutes, 120 minutes and 180 minutes respectively. The results are shown in FIG. 2. Therefore, in the whole adding process, the doped perovskite nanocrystalline keeps monodispersity and original morphology, and compared with the undoped perovskite nanocrystalline, the doped perovskite nanocrystalline prepared by the method has excellent high-temperature morphology stability.
Example 3
This example demonstrates that doped perovskite nanocrystals prepared according to the method of the present invention have good morphological stability at high temperatures.
1. Weighing Cs (CH)3COOH) powder 0.12 g, oleic acid 0.3 ml, octadecene 5ml were charged into a 25ml three-necked flask. Wherein Cs (CH)3COOH) and oleic acid in a molar ratio of 1: 1.5, the molar concentration of cesium ions is 0.12 mmol/ml. And introducing nitrogen while magnetically stirring, deoxidizing for 30 minutes, heating the flask to 150 ℃, keeping for 30 minutes to obtain a light yellow transparent cesium precursor solution, and keeping the temperature at 150 ℃ for later use.
2. Weighing PbCl20.069 g of powder, 0.5 ml of oleic acid, 0.5 ml of oleylamine and 5ml of octadecene were charged into a 25ml three-necked flask. Wherein PbCl2And oleic acid in a 1: 1, the molar ratio of oleic acid to oleylamine is 1.08: 1. the molar concentration of lead ions was 0.4 mmol/ml. Introducing nitrogen while magnetically stirring, removing oxygen for 30 min, heating to 195 deg.C, and maintaining for 20 min to obtain light yellowTransparent lead precursor solution, keeping the temperature of the system at 195 ℃ for standby.
3. 0.125 g of MnCl is weighed2Mixed with 5ml octadecene, 0.5 ml oleic acid and 0.5 ml oleylamine and charged into a 25ml three-necked flask. Wherein, MnCl2The molar ratio to oleic acid was 1: 1.5, the molar ratio of oleic acid to oleylamine is 1.08: 1, the molar concentration of manganese ions is 0.17 mmol/ml. Introducing nitrogen under magnetic stirring, deoxidizing for 30 minutes, heating to 150 ℃, preserving heat for 30 minutes, and then reducing the system temperature to 100 ℃ to obtain a manganese precursor solution for later use.
4. And then, quickly adding 0.4 ml of cesium precursor solution into the lead precursor solution, reacting for 1 minute to obtain a perovskite nanocrystalline mother solution, then adding 0.5 ml of manganese precursor solution, reacting for 30 minutes, and quickly cooling to room temperature to obtain a perovskite nanocrystalline doped crude solution.
5. And (3) carrying out centrifugal purification on the obtained perovskite nanocrystalline crude solution for 5 minutes, wherein the centrifugal rotating speed is 3000 r/min. And dissolving the collected nano-crystals in octadecene to obtain a perovskite nano-crystal solution.
6. After heating the doped perovskite nanocrystalline solution to 180 ℃, sampling and observing the evolution of the morphology at high temperature in 1 minute, 60 minutes, 120 minutes and 180 minutes respectively. The results are shown in FIG. 3. Therefore, in the whole adding process, the doped perovskite nanocrystalline keeps monodispersity and original morphology, and compared with the undoped perovskite nanocrystalline, the doped perovskite nanocrystalline prepared by the method has excellent high-temperature morphology stability.
The foregoing is only a preferred embodiment of the present invention and it should be noted that modifications and variations can be made by those skilled in the art without departing from the principle of the present invention and these modifications and variations should also be considered as the protection scope of the present invention.
Claims (8)
1. A preparation method of perovskite nanocrystalline with stable morphology at high temperature is characterized by comprising the following steps:
(1) mixing Cs (CH)3COOH), octadecene and oleic acidHeating for 20-60min at the temperature of 140-160 ℃ in a protective atmosphere to obtain a cesium precursor solution, and keeping the temperature of 120-160 ℃ for standby;
(2) dissolving lead halide in a mixture of octadecene, oleic acid and oleylamine at 180-200 ℃ under a protective atmosphere to obtain a lead precursor solution, and keeping the lead precursor solution at 180-200 ℃ for later use;
(3) dissolving doped metal halide in a mixture of octadecene, oleic acid and oleylamine at a high temperature of 150-180 ℃ under a protective atmosphere for reacting for 20-60min to obtain a transparent doped metal precursor solution, and keeping the temperature at 80-130 ℃ for later use;
(4) injecting the cesium precursor solution in the step (1) into the lead precursor solution in the step (2), reacting for 1-5min to obtain a perovskite nanocrystalline mother solution, injecting the doped metal precursor solution in the step (3) into the perovskite nanocrystalline mother solution, and reacting for 5-180 min to obtain a nanocrystalline solution;
(5) and (4) carrying out centrifugal purification on the nanocrystalline solution obtained in the step (4) under the condition of 3000 r/min, and dissolving the nanocrystalline precipitate in a nonpolar solvent to obtain the perovskite nanocrystalline with stable appearance at high temperature.
2. The method according to claim 1, wherein Cs (CH) in the step (1)3COOH) and oleic acid at a molar ratio of 1: 1.5-1: 3; the Cs (CH)3COOH) in octadecene and oleic acid at a molar concentration of 0.05-0.15 mmol/ml.
3. The method according to claim 1, wherein the molar ratio of the lead halide to the oleic acid in the step (2) is 1: 1-1: and 2, the molar ratio of the oleic acid to the oleylamine is 1: 0.75-1: 1.5, the molar concentration of the lead halide in the mixture of octadecene, oleic acid and oleylamine is 0.05-0.15 mmol/ml.
4. The method according to claim 1, wherein the molar ratio of the metal halide to the oleic acid in the doping in the step (3) is 1: 1-1: 2; the mol ratio of oleic acid to oleylamine was 1: 0.8-1: 1.2, the molar concentration of the metal-doped halide in the mixture of octadecene, oleic acid and oleylamine is 0.2-0.8 mmol/ml.
5. The method according to claim 1, wherein the metal halide is ZnX as the dopant in the step (3)2、MgX2、CaX2Or MnX2Wherein X = Cl, Br or I.
6. The method according to claim 1, wherein the reaction temperature in the step (4) is 180 to 200 ℃.
7. The preparation method according to claim 1, wherein the molar ratio of the doping metal in the doping metal precursor solution to the lead ions in the perovskite nanocrystalline mother solution in step (4) is 1: 0.5-1: 5.
8. the perovskite nanocrystal with stable morphology at high temperature prepared by the preparation method as claimed in claim 7.
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| CN115161025A (en) * | 2022-07-05 | 2022-10-11 | 中国科学院上海光学精密机械研究所 | Method for preparing superlattice microcavity by self-assembly of bromine-chlorine doped perovskite quantum dots |
| CN115612492A (en) * | 2022-11-10 | 2023-01-17 | 吉林大学 | Preparation method and application of high-entropy alloy-doped perovskite nanocrystalline synthesized at room temperature |
| CN115612492B (en) * | 2022-11-10 | 2023-09-26 | 吉林大学 | Preparation method and application of high-entropy alloy doped perovskite nanocrystalline synthesized at room temperature |
| CN116478690A (en) * | 2023-04-23 | 2023-07-25 | 天津大学 | Stable perovskite nanocrystalline based on novel ligand and preparation method thereof |
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