CN114906872A - Stably dispersed all-inorganic CsPbBr 3 Preparation method of perovskite nanorod - Google Patents

Stably dispersed all-inorganic CsPbBr 3 Preparation method of perovskite nanorod Download PDF

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CN114906872A
CN114906872A CN202210407839.1A CN202210407839A CN114906872A CN 114906872 A CN114906872 A CN 114906872A CN 202210407839 A CN202210407839 A CN 202210407839A CN 114906872 A CN114906872 A CN 114906872A
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CN114906872B (en
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王连军
胡晓博
周蓓莹
王建成
黄平
江莞
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Donghua University
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Abstract

The invention discloses a stably dispersed fully inorganic CsPbBr 3 The preparation method of the perovskite nanorod comprises the following steps: reacting PbBr 2 And CsOAc are respectively dissolved in DMF, and the mixture is stirred until the mixture is completely dissolved to obtain PbBr 2 Precursor and CsOAc solution; sequentially adding oleic acid, alkylamine and alkyl mercaptan into the CsOAc solution to obtain a CsOAc precursor; at room temperature, adding PbBr 2 Sequentially injecting the precursor and the CsOAc precursor into an anti-solvent, stirring to completely react, removing supernatant through centrifugation, adding a dispersing agent to re-disperse and precipitate, centrifuging again, and extracting the supernatant to obtain CsPbBr 3 Perovskite nanorod solution. The raw materials needed by the invention are cheap and easily available, the preparation method is simple, convenient and quick, and the prepared CsPbBr 3 The perovskite nanorod has good dispersibility and excellent stability.

Description

Stably dispersed all-inorganic CsPbBr 3 Preparation method of perovskite nanorod
Technical Field
The invention relates to stably dispersed fully inorganic CsPbBr 3 A perovskite nanorod and a preparation method thereof, belonging to the technical field of semiconductor nano-material preparation.
Background
Compared with the traditional fluorescent material, the perovskite nanocrystal has good application prospect in the fields of solar cells, light-emitting diodes, photoelectric detectors and lasers due to the excellent photoelectric properties such as good adjustability of light-emitting wavelength, high light-emitting efficiency, narrow light-emitting spectral line and the like, and becomes a current research hotspot. Perovskite materials are classified into organic-inorganic hybrid perovskites and all-inorganic perovskites according to the kind of constituent ions; the organic-inorganic hybrid perovskite material mainly comprises MAPbX 3 And FAPBX 3 (X ═ C1, Br, I), which is commonly used as an absorption layer of solar cells because of its small band gap value, absorption spectrum covering the visible region, and also having high electron and hole mobilities; in addition, organic-inorganic hybrid perovskite materials have good light emitting properties, and thus are also applied to light emitting diodes. However, the materials contain organic cations, so that the stability of the materials is poor, and the application of the materials in the fields of solar cells and luminescence is limited to a certain extent.
In recent years, fully inorganic CsPbX 3 The (X ═ C1, Br, I) perovskite nanocrystalline material has the characteristics of high fluorescence quantum yield, basically covering visible light region with emission wavelength, long carrier diffusion distance, simple synthesis method, low preparation cost and the like, and gradually attracts the wide attention of the scientific and industrial fields. In addition, compared with organic-inorganic hybrid perovskite nanocrystals, the all-inorganic perovskite nanocrystals do not contain organic cations, so that the all-inorganic perovskite nanocrystals have higher stability and have wider application prospects in the fields of light-emitting diodes, solar cells, lasers and photodetectors. Because the photoelectric property of the semiconductor nanocrystal is closely related to the shape and the size, the fully inorganic CsPbX with different shapes is realized 3 The controllable synthesis of (X ═ C1, Br, I) perovskite nanocrystals and the elucidation of the intrinsic link between their morphology and their optoelectronic properties are crucial to driving the commercial application of perovskite nanocrystals.
Compared with a three-dimensional perovskite nanocube, the one-dimensional nanorod has the advantage of controllable length (reaching micron level), can promote the transmission of photon-generated carriers in perovskite, and has great application potential in the fields of photoelectric detectors, solar cells and the like. At present, the all-inorganic perovskite nanorod is mainly prepared by a hot injection method and a microwave method, and has the defects of harsh experimental conditions, high preparation cost, incapability of realizing large-scale synthesis and the like. Therefore, the development of a simple, convenient and efficient large-scale preparation process of the high-performance all-inorganic perovskite nanorod is urgently needed.
Disclosure of Invention
The invention aims to solve the technical problems that: provides a stably dispersed fully inorganic CsPbBr 3 Perovskite nano-rod and its preparation method.
In order to solve the technical problems, the invention is realized by the following technical scheme:
stably dispersed all-inorganic CsPbBr 3 The preparation method of the perovskite nanorod comprises the following steps:
step 1): reacting PbBr 2 And CsOAc are respectively dissolved in DMF, and the mixture is stirred until the mixture is completely dissolved to obtain PbBr 2 Precursor and CsOAc solution;
step 2): sequentially adding oleic acid, alkylamine and alkyl mercaptan into the CsOAc solution to obtain a CsOAc precursor;
step 3): at room temperature, adding PbBr 2 Sequentially injecting the precursor and the CsOAc precursor into an anti-solvent, stirring to completely react, removing supernatant through centrifugation, adding a dispersing agent to re-disperse and precipitate, centrifuging again, and extracting the supernatant to obtain CsPbBr 3 Perovskite nanorod solution.
Preferably, in the step 1), PbBr 2 And the concentration of the solution formed by dissolving CsOAc in DMF is 0.02-0.08 mol/L.
Preferably, in the step 2), the alkylamine is any one of octylamine, dodecylamine and oleylamine.
Preferably, in the step 2), the alkyl mercaptan is any one of octyl mercaptan, dodecyl mercaptan, hexadecyl mercaptan and octadecyl mercaptan.
Preferably, in the step 2), the molar ratio of the alkylamine to the alkyl mercaptan is 4-10: 1, and the molar ratio of the oleic acid to the cesium acetate is 10-20.
Preferably, in the step 3), PbBr is added 2 The volume ratio of the precursor to the CsOAc precursor is 1-4: 1.
Preferably, in the step 3), the anti-solvent is toluene or ethyl acetate.
Preferably, in the step 3), the dispersant is chloroform, n-hexane or cyclohexane.
The invention utilizes the above-mentioned all-inorganic CsPbBr 3 The product prepared by the preparation method of the perovskite nanorod is nanorod in shape and has good dispersibility, the average length of the product is 41.4-48.7 nm, and the average diameter of the product is 3.7-6.5 nm.
Compared with the prior art, the invention has the following beneficial effects:
(1) PbBr required by the invention 2 The CsOAc precursor can be prepared in advance at room temperature, complex processes such as heating and the like are not needed, and the synthesis efficiency of the all-inorganic perovskite nanocrystal is greatly improved;
(2) the invention realizes the full inorganic CsPbBr by changing the dosage ratio of alkylamine and alkylthiol ligand 3 The perovskite nanorod is efficiently and controllably prepared, the obtained nanorod solution has good storage stability, can be stored for more than 45 days at normal temperature, and has good application prospect in the photoelectric field.
(3) The method has the advantages of simple and easily obtained raw materials, mild reaction conditions, simple and efficient operation, no need of experimental conditions such as high temperature and inert atmosphere protection, low preparation cost and suitability for large-scale industrial production.
Drawings
FIGS. 1 and 2 show CsPbBr prepared in example 1 3 Transmission electron microscope photos of the perovskite nano rod with different multiples;
FIG. 3 is CsPbBr prepared in example 1 3 The distribution diagram of the length of the perovskite nano rod is shown;
FIG. 4 shows CsPbBr prepared in example 1 3 X-ray diffraction pattern of perovskite nano rod;
FIG. 5 shows CsPbBr prepared in example 1 3 Of perovskite nanorodsAbsorption spectra and photoluminescence spectra;
FIG. 6 is CsPbBr prepared in example 1 3 A line graph of change in luminescence intensity of the perovskite nanorods stored at room temperature for 45 days;
FIG. 7 is CsPbBr prepared in example 2 3 Transmission electron microscope photographs of the perovskite nanorods;
FIG. 8 is CsPbBr prepared in example 3 3 Transmission electron microscope photographs of the perovskite nanorods;
FIG. 9 is CsPbBr prepared in example 4 3 Transmission electron microscope photographs of the perovskite nanorods;
FIG. 10 is CsPbBr prepared in example 5 3 And (3) transmission electron microscope photos of the perovskite nanorods.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
Stably dispersed all-inorganic CsPbBr 3 The preparation method of the perovskite nanorod comprises the following steps:
(1) 0.4mmol of PbBr was weighed separately 2 And 0.2mmol CsOAc powder in a beaker, then adding 10mL and 5mL DMF solution respectively, stirring and dissolving completely to obtain PbBr 2 Precursor and CsOAc solution;
(2) sequentially adding 1.1mL of oleic acid, 0.13mL of octylamine and 0.02mL of octylmercaptan into the CsOAc solution to obtain a CsOAc precursor;
(3) 0.32mL of PbBr was added at room temperature 2 And 0.16mL of CsOAc precursor are sequentially injected into 20mL of anti-solvent ethyl acetate, stirred to completely react, centrifuged for 5min under the condition of 9000r/min to remove supernatant, then 5mL of dispersant n-hexane is added into the precipitate for re-centrifugation, and the supernatant is extracted to obtain the all-inorganic CsPbBr 3 Perovskite nanorod solution.
The prepared fully inorganic CsPbBr 3 The transmission electron microscope photographs of the perovskite nanorods with different multiples are shown in figures 1 and 2, which indicate that the CsPbBr is successfully prepared 3 Nanorods and has better dispersibility, FIG. 3 is the distribution diagram of the particle size of the nanorodsThe average length is 41.4nm, and the average diameter is 5.8 nm; FIG. 4 is an X-ray diffraction pattern thereof, showing that CsPbBr was prepared 3 The nano-rods are in an orthogonal phase structure; FIG. 5 shows absorption and photoluminescence spectra, with CsPbBr appearing at 505nm and 515nm, respectively 3 Further demonstrates that this example synthesizes a pure phase of CsPbBr 3 Perovskite nanorods; FIG. 6 is a graph showing the variation of the luminescence intensity and peak position of nanorods with storage time, and the prepared fully inorganic CsPbBr was stored at 25 ℃ and 70% relative humidity for 45 days 3 The perovskite nanorod solution can still keep more than 80% of the initial fluorescence intensity, and the luminescence peak position of the perovskite nanorod solution does not fluctuate obviously, which indicates that the synthesized all-inorganic perovskite nanorod has higher stability.
Example 2
The present embodiment is different from embodiment 1 in that: in the step (2), 1.1mL of oleic acid, 0.077g of dodecylamine and 0.02mL of dodecyl mercaptan are sequentially added into the organic solution of CsOAc to obtain a CsOAc precursor solution;
FIG. 7 shows the fully inorganic CsPbBr prepared as described above 3 The transmission electron microscope photo of the perovskite nanorod shows that CsPbBr can be prepared by taking dodecylamine and dodecyl mercaptan as ligands 3 The perovskite nanorod has the average length of 48.7nm and the average diameter of 3.9nm and has better dispersity.
Example 3
The present embodiment is different from embodiment 1 in that: in the step (2), 1.0mL of oleic acid, 0.039mL of oleylamine and 0.01mL of octadecanethiol are sequentially added into the organic solution of CsOAc to obtain a CsOAc precursor solution;
FIG. 8 shows the total inorganic CsPbBr prepared in this example 3 Transmission electron microscope photographs of perovskite nanorods show that CsPbBr can be prepared by using oleylamine and octadecanethiol as ligands and properly reducing the use amount of oleic acid 3 The perovskite nanorod has the average length of 47.2nm, the average diameter of 3.7nm and better dispersity.
Example 4
The present embodiment is different from embodiment 1 in that: in the step (2), 0.8mL of oleic acid, 0.2mL of octylamine and 0.05mL of hexadecyl mercaptan are sequentially added to the organic solution of CsOAc to obtain a CsOAc precursor solution.
The prepared fully inorganic CsPbBr 3 The transmission electron micrograph of the perovskite nanorod is shown in FIG. 9, which shows that CsPbBr can be prepared by using octylamine and hexadecyl mercaptan as ligands and properly reducing the use amount of oleic acid 3 The perovskite nanorod has the average length of 45.7nm, the average diameter of 6.3nm and good dispersibility.
Example 5
The present embodiment is different from embodiment 1 in that: in step (3), PbBr 2 And CsOAc precursor in an amount of 0.48mL and 0.16mL, respectively, and the anti-solvent is toluene.
The prepared fully inorganic CsPbBr 3 The transmission electron micrograph of the perovskite nanorod is shown in FIG. 10, which shows that CsPbBr can be successfully prepared by changing the dosage ratio of the lead halide and the cesium acetate precursor 3 The perovskite nanorod has the average length of 43.7nm, the average diameter of 6.5nm and good dispersibility.
Example 6
The present embodiment is different from embodiment 1 in that: in the step (3), the dispersant of the perovskite nanocrystal is chloroform.
The obtained fully inorganic CsPbBr 3 The perovskite nanorods also can be uniformly dispersed in chloroform, the average length of the nanorods is 47.9nm, and a remarkable luminescence peak exists at 518 nm.
Example 7
The present embodiment is different from embodiment 1 in that: in the step (3), the dispersant is cyclohexane.
The obtained fully inorganic CsPbBr 3 The perovskite nano-rod can be uniformly dispersed in cyclohexane, the average length of the nano-rod is 45.3nm, and a luminous peak is obvious at 517 nm.

Claims (8)

1. Stably dispersed all-inorganic CsPbBr 3 The preparation method of the perovskite nanorod is characterized by comprising the following steps:
step 1): PbB will be mixedr 2 And CsOAc are respectively dissolved in DMF, and the mixture is stirred until the mixture is completely dissolved to obtain PbBr 2 Precursor and CsOAc solution;
step 2): sequentially adding oleic acid, alkylamine and alkyl mercaptan into the CsOAc solution to obtain a CsOAc precursor;
step 3): at room temperature, adding PbBr 2 Sequentially injecting the precursor and the CsOAc precursor into an anti-solvent, stirring to completely react, removing supernatant through centrifugation, adding a dispersing agent to re-disperse and precipitate, centrifuging again, and extracting the supernatant to obtain CsPbBr 3 Perovskite nanorod solution.
2. The stably dispersed all-inorganic CsPbBr of claim 1 3 The preparation method of the perovskite nanorod is characterized in that in the step 1), PbBr is added 2 And the concentration of the solution formed by dissolving CsOAc in DMF is 0.02-0.08 mol/L.
3. The stably dispersed all-inorganic CsPbBr of claim 1 3 The preparation method of the perovskite nanorod is characterized in that in the step 2), the alkylamine is any one of octylamine, dodecylamine and oleylamine.
4. A stably dispersed all-inorganic CsPbBr according to claim 1 3 The preparation method of the perovskite nanorod is characterized in that in the step 2), the alkyl mercaptan is any one of octyl mercaptan, dodecyl mercaptan, hexadecyl mercaptan and octadecyl mercaptan.
5. The stably dispersed all-inorganic CsPbBr of claim 1 3 The preparation method of the perovskite nanorod is characterized in that in the step 2), the molar ratio of alkylamine to alkyl mercaptan is 4-10: 1, and the molar ratio of oleic acid to cesium acetate is 10-20.
6. The stably dispersed all-inorganic CsPbBr of claim 1 3 The preparation method of the perovskite nanorod is characterized in that in the step 3), PbBr is added 2 The volume ratio of the precursor to the CsOAc precursor is 1-4: 1.
7. The stably dispersed all-inorganic CsPbBr of claim 1 3 The preparation method of the perovskite nanorod is characterized in that in the step 3), the anti-solvent is toluene or ethyl acetate.
8. The stably dispersed all-inorganic CsPbBr of claim 1 3 The preparation method of the perovskite nanorod is characterized in that in the step 3), the dispersing agent is chloroform, normal hexane or cyclohexane.
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CN116285990A (en) * 2023-03-10 2023-06-23 合肥工业大学 Method for preparing antimony doped cesium yttrium chloride lead-free perovskite luminescent material by room temperature anti-solvent precipitation method

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CN116285990B (en) * 2023-03-10 2024-01-30 合肥工业大学 Method for preparing antimony doped cesium yttrium chloride lead-free perovskite luminescent material by room temperature anti-solvent precipitation method

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