CN110437827A - A kind of blue light full-inorganic CsPbBrxCl3-xThe Morphological control method of perovskite nanometer sheet - Google Patents
A kind of blue light full-inorganic CsPbBrxCl3-xThe Morphological control method of perovskite nanometer sheet Download PDFInfo
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Abstract
The invention discloses a kind of blue light full-inorganic CsPbBrxCl3‑xThe Morphological control method of perovskite nanometer sheet.Preparation method is: first preparing oleic acid caesium presoma；Lead source presoma is prepared again, and finally caesium source presoma is injected into the precursor solution of lead source and obtains blue light full-inorganic CsPbBrxCl3‑xPerovskite nanometer sheet.When the injection rate in caesium source is 0.8 ± 0.1mL, the perovskite overwhelming majority of synthesis is the nanometer sheet of vertical direction；It is nanocrystalline when injection rate is 0.2~0.7mL；When injection rate is 0.9~2mL, vertical nanometer sheet is reduced, and horizontal nanometer sheet quantity increases.The invention has the advantages that the pattern of nanometer sheet can be regulated and controled by the injection rate for changing caesium source.The methods of different ligands, change oleic acid and the ratio of oleyl amine, control synthesis temperature are compared in the Morphological control technology reported at present, Morphological control method of the invention is easy to operate, can directly be achieved the purpose that by changing the injection rate in caesium source to perovskite nanometer sheet Morphological control.
Description
Technical field
The present invention relates to photoelectric display illumination technical field of nano material, and in particular to a kind of pattern tune of nanocrystal
Prosecutor method more particularly to a kind of blue light full-inorganic CsPbBrxCl3-xThe Morphological control method of perovskite nanometer sheet.
Background technique
The successful synthesis of last century Colloidal Quantum Dots (Quantum Dots) opens one for the development of low-dimensional quantum material
Fan new gate.Due to the presence of the quantum confined effect on three dimension scale, the energy level of quantum dot is distributed big with its size
It is small closely related.Therefore, researcher is the photoelectricity spy that this material is adjusted by regulating and controlling the size of quantum dot mostly at present
Property, and in addition to this, regulated and controled by further growth, adjust the pattern of material, we can obtain only in two-dimentional scale or one
Tie up the material on scale with quantum confined effect, it may be assumed that quantum rod (Quantum Rods) or nanometer sheet
(Nanoplatelets).Wherein, nanometer sheet material is due to only in one dimension by quantum confined effect, compared to quantum
Point, the spectrum of nanometer sheet show more obvious exciton absorption peak and narrower exciting light half-peak breadth (about 10nm), therefore, if
Nanometer sheet is applied in display device, we will obtain purer display color.
Two dimension (2D) APbX with accurate adjustable thickness3Nanocrystal is because of its unique property, especially quantum confinement
Effect and be considered as high-performance optical electronic device promising candidate.Although the preparation of 2D nanometer sheet achieves progress,
But still there are some challenges.Such as, it usually needs complicated and cumbersome step obtains the nanometer sheet of uniform-dimension, Er Qiewen
That offers middle report has using different ligands, the ratio of change oleic acid and oleyl amine, control synthesis temperature etc.
CsPbBrxCl3-xThe pattern of nanometer sheet, these are to CsPbX3The method of the Morphological control of nanometer sheet is mostly more complicated and troublesome.
Summary of the invention
The purpose of the present invention is to provide a kind of blue light full-inorganic CsPbBrxCl3-xThe Morphological control side of perovskite nanometer sheet
Method, the amount by adjusting injection caesium source reach the full-inorganic CsPbBr to synthesisxCl3-xThe mesh of perovskite nanometer sheet Morphological control
's.
Synthesis step of the invention are as follows:
A), caesium source presoma 1 is prepared
By 0.1620~0.1635g caesium source, 0.45~0.5mL oleic acid and 7~8mL octadecylene (ODE) are added to 25mL's
In three-necked flask, logical nitrogen circulation 1h is vacuumized at 120 DEG C, be then heated to 140 DEG C until solution become colorless it is transparent, so
Spare, as oleic acid caesium presoma 1 is kept the temperature at 100 DEG C afterwards.
B), lead source presoma 2 is prepared
It is 0.376mol by molal quantity total amount, weighs lead bromide (PbBr respectively2) and lead chloride (PbCl2), with 9~10mL
Octadecylene (ODE) is added in the three-necked flask of 50mL together and stirs evenly, and logical nitrogen circulation 15min is vacuumized at 110 DEG C,
Then 0.8~1mL oleic acid (OA) and 0.8~1mL oleyl amine (OLA) is added, continuation vacuumizes logical nitrogen circulation 1h at 110 DEG C,
Then lead to nitrogen, obtain lead source presoma 2.
C), CsPbBr is synthesizedxCl3-xPerovskite nanometer sheet
The temperature of lead source presoma 2 is raised to 150~170 DEG C, injects 0.2~2mL caesium source presoma 1, reaction 5 thereto
~10s, then horse back ice-water bath is cooled to room temperature, and finally obtains full-inorganic CsPbBrxCl3-xPerovskite nanometer sheet；
When the injection rate in caesium source is 0.8 ± 0.1mL, the perovskite overwhelming majority of synthesis is the nanometer sheet of vertical direction；
When the injection rate in caesium source is 0.2~0.7mL, the perovskite overwhelming majority of synthesis is nanocrystalline；When the injection rate in caesium source is 0.9
When~2mL, the quantity of the nanometer sheet of the perovskite vertical direction of synthesis is reduced, and the nanometer sheet quantity of horizontal direction increases.
The caesium source is cesium carbonate；
The lead source is lead bromide and lead chloride.
The present invention reaches the full-inorganic CsPbBr to synthesis by adjusting the amount in injection caesium sourcexCl3-xPerovskite nanometer sheet shape
The purpose of looks regulation.When the injection rate in caesium source is 0.8 ± 0.1mL, the perovskite overwhelming majority of synthesis is receiving for vertical direction
Rice piece；When the injection rate in caesium source is 0.2~0.7mL, the perovskite overwhelming majority of synthesis is nanocrystalline；When the injection rate in caesium source
When for 0.9~2mL, the quantity of the nanometer sheet of the perovskite vertical direction of synthesis is reduced, and the nanometer sheet quantity of horizontal direction increases.
In addition, having in existing Morphological control technology at present using different ligands, the ratio of change oleic acid and oleyl amine, control
Synthesis temperature processed etc. regulates and controls CsPbBrxCl3-xThe pattern of nanometer sheet.Compared to existing method, Morphological control method of the invention
It is easy to operate, can directly it be achieved the purpose that by changing caesium source injection rate to perovskite nanometer sheet Morphological control.
Detailed description of the invention
Fig. 1 is the luminescence generated by light and abosrption spectrogram for the perovskite nanometer sheet that embodiment 1 and embodiment 4 synthesize；
Fig. 2 is the transmission electron microscope figure for the perovskite nanometer sheet that embodiment 1 and embodiment 4 synthesize；
Fig. 3 is the photoluminescence spectra figure for the perovskite nanometer sheet that embodiment 2 and embodiment 5 synthesize；
Fig. 4 is the transmission electron microscope figure for the perovskite nanometer sheet that embodiment 2 and embodiment 5 synthesize；
Fig. 5 is the photoluminescence spectra figure for the perovskite nanometer sheet that embodiment 3 and embodiment 6 synthesize；
Fig. 6 is the transmission electron microscope figure for the perovskite nanometer sheet that embodiment 3 and embodiment 6 synthesize.
Specific embodiment
With embodiment, the present invention is further described below.
Embodiment 1:
A), caesium source presoma 1 is prepared
By 0.1628g cesium carbonate (Cs2CO3), 0.5mL oleic acid and 8mL octadecylene (ODE) are added to the three-necked flask of 25mL
In, logical nitrogen circulation 1h is vacuumized at 120 DEG C, be then heated to 140 DEG C until solution become colorless it is transparent, then 100
Spare, as oleic acid caesium presoma 1 is kept the temperature at DEG C.
B), lead source presoma 2 is prepared
By 0.0966g (0.2632mmol) lead bromide (PbBr2), 0.0314g (0.1128mmol) lead chloride (PbCl2) and
10mL ODE is added in the three-necked flask of 50mL, and logical nitrogen circulation 15min is vacuumized at 110 DEG C, and 1mL oleic acid is then added
With 1mL oleyl amine, continuation vacuumizes logical nitrogen circulation 1h at 110 DEG C, then leads to nitrogen and obtains lead source presoma 2.
C), CsPbBr is synthesizedxCl3-xPerovskite nanometer sheet
The temperature of lead source presoma 2 is raised to 150 DEG C, injects 0.8mL caesium source, reacts 5s, then horse back ice-water bath is cooling
To room temperature, full-inorganic CsPbBr is finally obtainedxCl3-xPerovskite nanometer sheet.
Synthesized sample is CsPbBr when caesium source injection rate is normal2.1Cl0.9Perovskite nanometer sheet, luminescence generated by light and
Abosrption spectrogram is referring to Fig. 1, and as Br:Cl=7:3, glow peak is in 466.51nm, and absorption peak is in 446nm；Its transmitted electron is aobvious
Referring to fig. 2, the perovskite overwhelming majority of synthesis is the nanometer sheet of vertical direction to micro mirror figure.
Embodiment 2:
The present embodiment is same as Example 1, and the caesium source injection rate in embodiment 1 is only changed to 0.4mL.
Synthesized sample is CsPbBr when caesium source injection rate is reduced2.1Cl0.9Perovskite nanometer sheet, luminescence generated by light light
Spectrogram is referring to Fig. 3, and as Br:Cl=7:3, glow peak is in 463.51nm；Its transmission electron microscope figure referring to fig. 4, synthesis
The perovskite overwhelming majority is nanocrystalline.
Embodiment 3:
The present embodiment is same as Example 1, and the caesium source injection rate in embodiment 1 is only changed to 1.6mL.
Synthesized sample is CsPbBr when caesium source injection rate increases2.1Cl0.9Perovskite nanometer sheet, luminescence generated by light light
Spectrogram is referring to Fig. 5, and as Br:Cl=7:3, glow peak is in 475.53nm；Its transmission electron microscope figure referring to Fig. 6, synthesis
The quantity of the nanometer sheet of perovskite vertical direction is reduced, and the nanometer sheet quantity of horizontal direction increases.
Embodiment 4:
A), caesium source presoma 1 is prepared
By 0.1628g cesium carbonate (Cs2CO3), 0.5ml oleic acid and 8mL octadecylene (ODE) are added to the three-necked flask of 25mL
In, logical nitrogen circulation 1h is vacuumized at 120 DEG C, be then heated to 140 DEG C until solution become colorless it is transparent, then 100
Spare, as oleic acid caesium presoma 1 is kept the temperature at DEG C.
B), lead source presoma 2 is prepared
By 0.069g (0.188mmol) lead bromide (PbBr2), 0.0522g (0.188mmol) lead chloride (PbCl2) and 10mL
ODE is added in the three-necked flask of 50mL, and logical nitrogen circulation 15min is vacuumized at 110 DEG C, and 1mL oleic acid and 1mL is then added
Oleyl amine, continuation vacuumize logical nitrogen circulation 1h at 110 DEG C, then lead to nitrogen and obtain lead source presoma 2.
C), CsPbBr is synthesizedxCl3-xPerovskite nanometer sheet
The temperature of lead source presoma 2 is raised to 150 DEG C, injects 0.8mL caesium source, reacts 5s, then horse back ice-water bath is cooling
To room temperature, full-inorganic CsPbBr is finally obtainedxCl3-xPerovskite nanometer sheet.
Synthesized sample is CsPbBr when caesium source injection rate is normal1.5Cl1.5Perovskite nanometer sheet, luminescence generated by light and
Abosrption spectrogram is referring to Fig. 1, and as Br:Cl=1:1, glow peak is in 449.21nm, and absorption peak is in 428nm；Its transmitted electron is aobvious
Referring to fig. 2, the perovskite overwhelming majority of synthesis is the nanometer sheet of vertical direction to micro mirror figure.
Embodiment 5:
The present embodiment is same as Example 3, and the caesium source injection rate in embodiment 3 is only changed to 0.4mL.
Synthesized sample is CsPbBr when caesium source injection rate is reduced1.5Cl1.5Perovskite nanometer sheet, luminescence generated by light light
Spectrogram is referring to Fig. 3, and as Br:Cl=1:1, glow peak is in 442.44nm；Its transmission electron microscope figure referring to fig. 4, synthesis
The perovskite overwhelming majority is nanocrystalline.
Embodiment 6:
The present embodiment is same as Example 3, and the caesium source injection rate in embodiment 3 is only changed to 1.6mL.
Synthesized sample is CsPbBr when caesium source injection rate increases1.5Cl1.5Perovskite nanometer sheet, luminescence generated by light light
Spectrogram is referring to Fig. 5, and as Br:Cl=1:1, glow peak is in 449.97nm；Its transmission electron microscope figure referring to Fig. 6, synthesis
The quantity of the nanometer sheet of perovskite vertical direction is reduced, and the nanometer sheet quantity of horizontal direction increases.
Claims (1)
1. a kind of blue light full-inorganic CsPbBrxCl3-xThe Morphological control method of perovskite nanometer sheet, it is characterised in that including following step
It is rapid:
A), caesium source presoma 1 is prepared
By 0.1620~0.1635g caesium source, 0.45~0.5mL oleic acid and 7~8mL octadecylene (ODE) are added to three mouthfuls of 25mL
In flask, logical nitrogen circulation 1h is vacuumized at 120 DEG C, is then heated to 140 DEG C until solution becomes colorless transparent, is then existed
Spare, as oleic acid caesium presoma 1 is kept the temperature at 100 DEG C；
B), lead source presoma 2 is prepared
It is 0.376mol by molal quantity total amount, weighs lead bromide (PbBr respectively2) and lead chloride (PbCl2), with 9~10mL 18
Alkene (ODE) is added in the three-necked flask of 50mL together and stirs evenly, and logical nitrogen circulation 15min is vacuumized at 110 DEG C, then
0.8~1mL oleic acid (OA) and 0.8~1mL oleyl amine (OLA) is added, continuation vacuumizes logical nitrogen circulation 1h at 110 DEG C, then
Logical nitrogen, obtains lead source presoma 2；
C), CsPbBr is synthesizedxCl3-xPerovskite nanometer sheet
The temperature of lead source presoma 2 is raised to 150~170 DEG C, thereto injection 0.2~2mL caesium source presoma 1, reaction 5~
10s, then horse back ice-water bath is cooled to room temperature, and finally obtains full-inorganic CsPbBrxCl3-xPerovskite nanometer sheet；
When the injection rate in caesium source is 0.8 ± 0.1mL, the perovskite overwhelming majority of synthesis is the nanometer sheet of vertical direction；Work as caesium
When the injection rate in source is 0.2~0.7mL, the perovskite overwhelming majority of synthesis is nanocrystalline；When caesium source injection rate be 0.9~
When 2mL, the quantity of the nanometer sheet of the perovskite vertical direction of synthesis is reduced, and the nanometer sheet quantity of horizontal direction increases；
The caesium source is cesium carbonate；
The lead source is lead bromide and lead chloride.
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| CN110943178A (en) * | 2019-11-25 | 2020-03-31 | 北京科技大学 | Self-assembly multi-dimensional quantum well CsPbX3Perovskite nanocrystalline electroluminescent diode |
| CN110982523A (en) * | 2019-12-11 | 2020-04-10 | 西南交通大学 | Copper-doped quasi-two-dimensional all-inorganic perovskite material and preparation method thereof |
| CN111031624A (en) * | 2019-12-27 | 2020-04-17 | 华中科技大学 | Method for stabilizing electroluminescent spectrum of mixed halogen perovskite material and application |
| CN111204797A (en) * | 2020-01-17 | 2020-05-29 | 南京工业大学 | Morphology-controllable all-inorganic CsPbBr3Preparation method of perovskite nanocrystal |
| CN111233030A (en) * | 2020-01-17 | 2020-06-05 | 南京工业大学 | Perovskite CsPbBr3Preparation method of nanosheet |
| CN111276623A (en) * | 2020-01-19 | 2020-06-12 | 中国工程物理研究院流体物理研究所 | Modified hole transport layer and blue-light perovskite light-emitting diode based on same |
| CN111661867A (en) * | 2020-06-30 | 2020-09-15 | 重庆大学 | Preparation method of lead-free cesium copper chloride nanocrystalline and product and application thereof |
| CN115418224A (en) * | 2022-07-31 | 2022-12-02 | 南京邮电大学 | Method for efficiently doping blue light luminescent material in divalent metal ion organic solution |
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| CN110943178A (en) * | 2019-11-25 | 2020-03-31 | 北京科技大学 | Self-assembly multi-dimensional quantum well CsPbX3Perovskite nanocrystalline electroluminescent diode |
| CN110982523A (en) * | 2019-12-11 | 2020-04-10 | 西南交通大学 | Copper-doped quasi-two-dimensional all-inorganic perovskite material and preparation method thereof |
| CN111031624A (en) * | 2019-12-27 | 2020-04-17 | 华中科技大学 | Method for stabilizing electroluminescent spectrum of mixed halogen perovskite material and application |
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| CN111276623A (en) * | 2020-01-19 | 2020-06-12 | 中国工程物理研究院流体物理研究所 | Modified hole transport layer and blue-light perovskite light-emitting diode based on same |
| CN111661867A (en) * | 2020-06-30 | 2020-09-15 | 重庆大学 | Preparation method of lead-free cesium copper chloride nanocrystalline and product and application thereof |
| CN111661867B (en) * | 2020-06-30 | 2022-04-29 | 重庆大学 | Preparation method of lead-free cesium copper chloride nanocrystalline and product and application thereof |
| CN115418224A (en) * | 2022-07-31 | 2022-12-02 | 南京邮电大学 | Method for efficiently doping blue light luminescent material in divalent metal ion organic solution |
| CN115418224B (en) * | 2022-07-31 | 2024-05-24 | 南京邮电大学 | Method for efficiently doping blue light luminescent material with divalent metal ion organic solution |
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