CN114196393B - Perovskite quantum dot for enhancing core-shell anchoring, preparation method and application - Google Patents
Perovskite quantum dot for enhancing core-shell anchoring, preparation method and application Download PDFInfo
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Abstract
The invention provides a perovskite quantum dot for enhancing core-shell anchoring, a preparation method and application thereof, wherein the preparation method comprises the following steps: and mixing the porous material, the benign solvent and the perovskite raw material to obtain a mixture, carrying out precipitation treatment after mixing to obtain the porous material with perovskite crystal nucleus, and preparing the perovskite quantum dot with the reinforced core-shell anchoring after heating treatment. The perovskite crystal lattice and the porous material form firm connection through chemical bonding by a two-step method of anchoring and then growing, so that the perovskite crystal lattice has the effects of stabilizing a crystal structure and improving stability. Meanwhile, the method has universality, is suitable for various solvents through a solution method pre-burying crystal nucleus process, and is easy to amplify and produce in mass.
Description
Technical Field
The invention belongs to the technical field of perovskite quantum dots, and relates to a perovskite quantum dot for enhancing core-shell anchoring, a preparation method and application thereof.
Background
With the popularization and development of quantum dot display technology, the requirements of people on the display performance, stability, environmental protection and other aspects of quantum dot materials are increasingly increased. Compared with the traditional semiconductor quantum dots, the lead halogen perovskite quantum dots provide possibility for mass production of high-performance optical devices due to the characteristics of excellent photoelectric performance, lower preparation cost, environmental friendliness and the like, and gradually become a powerful competitor in the display field.
However, due to the self-ionic crystal structure characteristics, the problems of thermal induced phase change, ion migration and the like, the lead-halogen perovskite quantum dot material is difficult to maintain good luminous efficiency for a long time under severe conditions such as moisture, oxygen, blue light, thermal atmosphere and the like, and the commercialized road of the lead-halogen perovskite quantum dot material is seriously influenced. In order to solve this problem, researchers have made a great deal of research on improving the stability of quantum dots. In general, quantum dot encapsulation technology is considered as one of the most effective means for improving stability, and perovskite quantum dots are encapsulated in an inert shell, so that the influence of moisture and oxygen environment can be effectively isolated, and meanwhile, ion exchange and loss are preventedThereby greatly improving the weather resistance and the service life of the quantum dot. On one hand, the encapsulation mode can be to synthesize perovskite quantum dots in advance, and then grow and clad inert materials on the surface of the perovskite quantum dots; on the other hand, the mesoporous material can be introduced into the perovskite quantum dot preparation process, so that the quantum dot grows in situ in the hole of the mesoporous material, and then the hole is closed to form a core-shell structure. For example, document (10.1002/adfm.201604782) reports a solution method for preparing polymer coated perovskite quantum dots, wherein pre-synthesized perovskite nanocrystals and polymers are dispersed in a solvent, and then the polymers are agglomerated and precipitated to form a core-shell structure, so that the perovskite quantum dot material resistant to water-oxygen environment and blue light is obtained. Document (10.1021/acterenylett.1c00052) reports the preparation of mesoporous SiO by the molten salt sintering process 2 Coated CsPbBr 3 Quantum dot, the melted precursor material is poured into mesoporous SiO 2 At the same time utilize molten NaNO 3 、KNO 3 And blocking the pore canal to form a coating structure, so as to obtain the quantum dot material which is stable in water and heat and can be produced in a large scale. SiO is reported in the literature (10.1038/s 41467-019-13881-0) 2 Molecular sieve encapsulated CsPbBr 3 The quantum dot is prepared by filling a precursor into a molecular sieve by using an aqueous solution, and collapsing the molecular sieve by heat treatment to realize encapsulation. Although perovskite quantum dot materials with certain stability can be obtained by a plurality of methods, the blue light stability and the thermal stability of the perovskite quantum dot materials are still quite different from the actual application, and the market demands cannot be met.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a perovskite quantum dot for enhancing core-shell anchoring, a preparation method and application thereof, and the problems that the crystal structure of the quantum dot is stabilized by combining the core shells of the quantum dot through chemical bonds in a mode of embedding crystal nuclei, and the crystal lattice distortion of the quantum dot is restrained under severe environments such as light, heat and the like so as to reduce the luminous efficiency are solved.
To achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method of preparing a perovskite quantum dot for enhancing core-shell anchoring, the method comprising:
dispersing the porous material, the collapsing agent and the perovskite raw material in a benign solvent to obtain a dispersion liquid, separating out the dispersion liquid to prepare the porous material with perovskite crystal nucleus, and heating to prepare the perovskite quantum dot with reinforced core-shell anchoring.
The invention combines the quantum dot core-shells through firm chemical bonds in a pre-buried crystal nucleus manner, plays a role in stabilizing the perovskite quantum dot crystal structure, and inhibits the problems of reducing luminous efficiency due to lattice distortion generated in severe environments such as light, heat and the like. Further, the process of pre-embedding crystal nucleus disperses perovskite precursor 'ion level' on hydroxyl sites on the surface of inorganic porous material by a solution method to form high-dispersion quantum dot crystal nucleus with uniform particle size distribution, so that the grown quantum dot has controllable size, uniform particle size and adjustable luminescence characteristic; the perovskite quantum dot material prepared by the method has good luminous efficiency and better resistance to harsh conditions such as water, oxygen, light, heat and the like.
As a preferred embodiment of the present invention, the benign solvent comprises one or a combination of at least two of dimethyl sulfoxide, N-dimethylformamide or N-methylpyrrolidone, and further preferably dimethyl sulfoxide.
In the present invention, the benign solvent, that is, the solvent capable of embedding the nucleus into the core-shell structure, may form hydroxyl sites on the inner wall of the shell, for example.
As a preferred embodiment of the present invention, the pore diameter of the porous material is not more than 20nm, for example, 1nm, 2nm, 4nm, 6nm, 8nm, 10nm, 12nm, 14nm, 16nm, 18nm or 20nm, and more preferably 3 to 10nm.
Preferably, the collapsing agent comprises potassium bromide.
It should be noted that, the invention uses inorganic porous materials with better light and heat stability as the protective layer, so as to avoid the problem of poor structural stability of the organic polymer, further prolong the service life of the perovskite quantum dot material, for example, the porous materials comprise inorganic porous materials, and the inorganic porous materials comprise one or a combination of at least two of MCM, SBA, ZSM, naY or Zeolite.
As a preferred embodiment of the present invention, a gap filler is added to the dispersion.
Preferably, the gap filling material comprises one or a combination of at least two of potassium nitrate, aluminum nitrate or eutectic system.
According to the invention, in the process of pre-burying crystal nucleus, gap filling materials are added to form chemical bonding with the surface of the quantum dot to passivate, so that the stability is further improved.
It should be noted that the definition of the eutectic system is: when the homogeneous solid mixture is heated to a certain temperature, it melts into a melt of the same composition, which melts at a temperature lower than the melting point of the compounds or elements, for example a low-melting glass frit, which has a melting temperature of 400-700 ℃.
As a preferable technical scheme of the invention, the mass ratio of the perovskite raw material to the porous material is 1 (1-10), for example, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9 or 1:10, and more preferably 1:3.
The mass ratio of the perovskite raw material to the porous material is controlled to be 1: if the ratio is lower than the mass ratio, (1-10) there is a problem that the quantum dots are small and the luminescence is incomplete, and if the ratio is higher than the mass ratio, (1-10) there is a problem that the crystal grain size is large and the luminescence efficiency is low.
As a preferred technical scheme of the invention, the perovskite raw material comprises green light quantum dots and/or red light quantum dots.
Preferably, the green light quantum dots comprise CsBr and PbBr 2 Or the bulk CsPbBr 3 Further preferred is the bulk CsPbBr 3 。
Preferably, the red light quantum dots comprise CsBr and PbI 2 Or the bulk CsPbBri 2 Further preferred are CsBr and PbI 2 。
As a preferable embodiment of the present invention, the perovskite raw material is additionally charged during the heat treatment.
According to the invention, perovskite raw materials are additionally added in the heat treatment process, so that the effective regulation and control of the grain size are realized, and the luminous characteristics are regulated and controlled.
Preferably, the perovskite feedstock is the bulk phase CsPbBr 3 The mass ratio of the additional input amount of the perovskite raw material to the porous material is 1: (1 to 10), for example, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9 or 1:10, and more preferably 1:5.
Preferably, the perovskite raw material is CsBr and PbI 2 Is additionally added into the perovskite raw material, csBr and PbI 2 The mass ratio of the porous material to the porous material is 1:2 (5-15), for example, 1:2:5, 1:2:6, 1:2:7, 1:2:8, 1:2:9, 1:2:10, 1:2:11, 1:2:12, 1:2:13, 1:2:14 or 1:2:15, and further preferably 1:2:8.
In a preferred embodiment of the present invention, the precipitation treatment includes heating precipitation or precipitation of a poor solvent, preferably precipitation of a poor solvent.
Preferably, the heating precipitation method includes: heating the mixed mixture, evaporating the solvent to dryness, and separating out the precursor material.
Preferably, the method for precipitating the poor solvent includes: and (3) dropwise adding a poor solvent into the mixed mixture, separating out a precursor material, and separating and drying.
Preferably, the poor solvent comprises an alcohol and/or toluene, and more preferably isopropanol.
In a preferred embodiment of the present invention, the temperature of the heat treatment is 350 to 1000 ℃, for example 350 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃, or 1000 ℃, more preferably 590 ℃.
Preferably, the heating rate of the heating treatment is 1 to 15℃per minute, for example, 1℃per minute, 2℃per minute, 3℃per minute, 4℃per minute, 5℃per minute, 6℃per minute, 7℃per minute, 8℃per minute, 9℃per minute, 10℃per minute, 11℃per minute, 12℃per minute, 13℃per minute, 14℃per minute or 15℃per minute, and more preferably 10℃per minute.
Preferably, the heat-preserving time of the heating treatment is 10 to 180min, for example, 10min, 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min, 120min, 130min, 140min, 150min, 160min, 170min or 180min, and more preferably 30min.
Illustratively, a method for preparing the perovskite quantum dot for enhancing core-shell anchoring is provided, which specifically comprises the following steps:
dispersing the porous material, the collapse agent and the perovskite raw material in a benign solvent to obtain a dispersion liquid, and separating out a precursor material by adopting a heating separation or dropwise adding a poor solvent separation mode to prepare the porous material with perovskite crystal nucleus;
heating the porous material with perovskite crystal nucleus at 350-1000 ℃ for 10-180 min, wherein the heating rate is 1-15 ℃/min, adding perovskite raw material in the heating treatment process, and regulating the grain size to prepare the perovskite quantum dot with reinforced core-shell anchoring.
In a second aspect, the invention provides a perovskite quantum dot with reinforced core-shell anchoring, the perovskite quantum dot with reinforced core-shell anchoring comprises a shell and a perovskite quantum dot core arranged in the shell, the perovskite quantum dot core is bonded and anchored with the shell, and the perovskite quantum dot with reinforced core-shell anchoring is prepared by the preparation method of the perovskite quantum dot with reinforced core-shell anchoring in the first aspect.
In a third aspect, the present invention provides the use of a reinforced core-shell anchored perovskite quantum dot according to the second aspect for an optoelectronic device.
The numerical ranges recited herein include not only the above-listed point values, but also any point values between the above-listed numerical ranges that are not listed, and are limited in space and for the sake of brevity, the present invention is not intended to be exhaustive of the specific point values that the stated ranges include.
Compared with the prior art, the invention has the beneficial effects that:
the invention combines the quantum dot core-shells through firm chemical bonds in a pre-buried crystal nucleus manner, plays a role in stabilizing the perovskite quantum dot crystal structure, and inhibits the problems of reducing luminous efficiency due to lattice distortion generated in severe environments such as light, heat and the like. Further, the process of pre-embedding crystal nucleus disperses perovskite precursor 'ion level' on hydroxyl sites on the surface of inorganic porous material by a solution method to form high-dispersion quantum dot crystal nucleus with uniform particle size distribution, so that the grown quantum dot has controllable size, uniform particle size and adjustable luminescence characteristic; the perovskite quantum dot material prepared by the method has good luminous efficiency and better resistance to harsh conditions such as water, oxygen, light, heat and the like.
Drawings
FIG. 1 is a schematic flow chart of a preparation method of a perovskite quantum dot with enhanced core-shell anchoring provided in example 1 of the present invention;
FIG. 2 is a comparative graph of the dry heat aging test of example 1 and comparative example 1 of the present invention;
FIG. 3 is a comparative chart of the blue aging test of example 1 and comparative example 1 of the present invention.
Detailed Description
For better illustrating the present invention, the technical scheme of the present invention is convenient to understand, and the present invention is further described in detail below. The following examples are merely illustrative of the present invention and are not intended to represent or limit the scope of the invention as defined in the claims.
In one embodiment, the invention provides a perovskite quantum dot with enhanced core-shell anchoring comprising an outer shell, and a perovskite quantum dot core disposed within the outer shell, the perovskite quantum dot core being bonded and anchored to the outer shell.
Example 1
The embodiment provides a preparation method of perovskite quantum dots for enhancing core-shell anchoring, as shown in fig. 1, the preparation method comprises the following steps:
0.1g of potassium bromide, 0.0667g of CsPbBr in the bulk phase 3 Dissolving in dimethyl sulfoxide, adding 0.2g of MCM-41 molecular sieve powder, and carrying out ultrasonic dispersion mixing, wherein the average pore diameter of the MCM-41 molecular sieve powder is 7 nm;
(II) dropwise adding 50ml of isopropanol into the mixed solution in the step (I) and continuously stirring to separate out yellow precipitate, centrifuging and drying the precipitate to obtain precursor powder;
(III) after uniformly grinding the precursor powder, carrying out heat treatment for 30min at 590 ℃ and heating up at a rate of 10 ℃/min, so as to prepare the reinforced core-shell anchored perovskite quantum dot.
Example 2
This example provides a method for preparing perovskite quantum dots with enhanced core-shell anchoring, which differs from example 1 in that the bulk phase CsPbBr 3 Replaced by 0.0245g CsBr and 0.0422g PbBr 2 The remaining steps and parameters are exactly the same as in example 1.
Example 3
The present example provides a method for preparing perovskite quantum dots with enhanced core-shell anchoring, which is different from example 1 in that 0.2g of potassium nitrate is added in step (i), and the rest steps and parameters are identical to those of example 1.
Example 4
This example provides a method for preparing perovskite quantum dots with enhanced core-shell anchoring, which is different from example 1 in that in step (I), the bulk phase CsPbBr is reacted 3 Replaced by 0.0211g CsBr and 0.0456g PbI 2 The remaining steps and parameters are exactly the same as in example 1.
Example 5
This example provides a method for preparing perovskite quantum dots with enhanced core-shell anchoring, which is different from example 1 in that in step (I), the following is carried outBulk CsPbBr 3 Replacement with the bulk CsPbBri 2 The remaining steps and parameters are exactly the same as in example 1.
Example 6
The present example provides a method for preparing perovskite quantum dots with enhanced core-shell anchoring, which is different from example 1 in that in step (i), the MCM-41 molecular sieve is replaced with the SBA-15 molecular sieve, and the remaining steps and parameters are identical to those of example 1.
Example 7
The embodiment provides a preparation method of perovskite quantum dots for enhancing core-shell anchoring, which comprises the following steps:
0.1g of potassium bromide and 0.1g of CsPbBr in bulk phase 3 Dissolving in dimethylformamide, adding 0.2g of ZSM powder, and carrying out ultrasonic dispersion and mixing;
(II) dropwise adding 50ml of toluene into the mixed solution in the step (I) and continuously stirring to separate out yellow precipitate, centrifuging and drying the precipitate to obtain precursor powder;
(III) after the precursor powder is ground uniformly, carrying out heat treatment for 100min at 350 ℃ and heating up at a rate of 1 ℃/min, so as to prepare the reinforced core-shell anchored perovskite quantum dot.
Example 8
The embodiment provides a preparation method of perovskite quantum dots for enhancing core-shell anchoring, which comprises the following steps:
0.1g of potassium bromide and 0.04g of CsPbBr in bulk phase 3 Dissolving in N-methyl pyrrolidone, adding 0.2g Zeolite powder, and performing ultrasonic dispersion mixing;
(II) heating the mixed solution in the step (I), and evaporating to dryness to obtain precursor powder;
(III) after the precursor powder is ground uniformly, carrying out heat treatment for 10min at 1000 ℃ and heating up at a rate of 15 ℃/min, so as to prepare the reinforced core-shell anchored perovskite quantum dot.
Example 9
The embodiment provides a preparation method of perovskite quantum dots for enhancing core-shell anchoring, which comprises the following steps:
(I) 0.1g of potassium bromide, 0.025g of CsBr, 0.05g of PbI 2 Dissolving in dimethyl sulfoxide, adding 0.2g NaY powder, and performing ultrasonic dispersion mixing;
(II) heating the mixed solution in the step (I), and evaporating to dryness to obtain precursor powder;
and (III) after uniformly grinding the precursor powder, carrying out heat treatment for 20min at 700 ℃, wherein the heating rate is 10 ℃/min, and preparing the reinforced core-shell anchored perovskite quantum dot.
Example 10
This example provides a method for preparing perovskite quantum dots, which differs from example 1 in that the bulk CsPbBr 3 The mass of (2) was 0.2g, and the rest of the steps and parameters were exactly the same as in example 1.
Example 11
This example provides a method for preparing perovskite quantum dots, which differs from example 1 in that the bulk CsPbBr 3 The mass of (2) was 0.02g, and the rest of the procedure and parameters were exactly the same as in example 1.
Example 12
The present example provides a method for preparing perovskite quantum dots, which is different from example 1 in that in step (III), 0.04g of bulk CsPbBr is additionally added during the heat treatment 3 The remaining steps and parameters are exactly the same as in example 1.
Comparative example 1
The comparative example provides a method for preparing perovskite quantum dots, which is different from the method in the embodiment 1 in that in the step (I), no pre-buried crystal nucleus is performed, and the method comprises the following steps:
adding 0.1g of potassium bromide into 25ml of deionized water, adding 0.2g of MCM-41 molecular sieve powder, carrying out ultrasonic dispersion mixing, and stirring at 150 ℃ until the water is completely evaporated to dryness;
(II) the product obtained in step (I) was combined with 0.0667g of CsPbBr in the bulk phase 3 Grinding, mixing, heat treating at 590 deg.C for 30min at a heating rate of 10deg.C/min to obtain the final productPerovskite quantum dots.
The perovskite quantum dots prepared in the above examples and comparative examples were subjected to performance tests including a dry heat aging test at 85 ℃ and a 447nm, 1000nit blue aging test, the test results being shown in table 1, wherein the dry heat aging test and the blue aging test of example 1 and comparative example 1 are shown in the pairs such as fig. 2 and 3.
TABLE 1
Compared with comparative example 1, it can be seen that the invention combines quantum dot core-shells through firm chemical bonds in a manner of embedding crystal nuclei, plays a role in stabilizing the crystal structure of perovskite quantum dots, and suppresses the problem that lattice distortion is generated in severe environments such as light, heat and the like to reduce luminous efficiency. Further, the process of pre-embedding crystal nucleus disperses perovskite precursor 'ion level' on hydroxyl sites on the surface of inorganic porous material by a solution method to form high-dispersion quantum dot crystal nucleus with uniform particle size distribution, so that the grown quantum dot has controllable size, uniform particle size and adjustable luminescence characteristic; the perovskite quantum dot material prepared by the method has good luminous efficiency and better resistance to harsh conditions such as water, oxygen, light, heat and the like.
The applicant declares that the above is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that are easily conceivable within the technical scope of the present invention disclosed by the present invention fall within the scope of the present invention and the disclosure.
Claims (14)
1. A method for preparing a perovskite quantum dot for enhancing core-shell anchoring, which is characterized by comprising the following steps:
dispersing a porous material, a collapse agent and a perovskite raw material in a benign solvent to obtain a dispersion liquid, adding a gap filling material into the dispersion liquid, performing precipitation treatment on the dispersion liquid to prepare a porous material with perovskite crystal nuclei, and performing heating treatment to prepare the perovskite quantum dots anchored by the reinforced core-shell;
the collapsing agent comprises potassium bromide; the benign solvent comprises one or a combination of at least two of dimethyl sulfoxide, N-dimethylformamide or N-methylpyrrolidone; the gap filling material comprises one or a combination of at least two of potassium nitrate, aluminum nitrate or a eutectic system;
the precipitation treatment mode is heating precipitation or precipitation by dripping poor solvent; the heating precipitation mode comprises the following steps: heating the mixed mixture, evaporating the solvent to dryness, and separating out a precursor material; the precipitation method of the poor solvent includes: and (3) dropwise adding a poor solvent into the mixed mixture, separating out a precursor material, and separating and drying.
2. The method according to claim 1, wherein the pore size of the porous material is 20nm or less.
3. The preparation method according to claim 1, wherein the mass ratio of the perovskite raw material to the porous material is 1 (1-10).
4. The method of claim 1, wherein the perovskite feedstock comprises green quantum dots and/or red quantum dots;
the green light quantum dots comprise CsBr and PbBr 2 Or the bulk CsPbBr 3 ；
The red light quantum dots comprise CsBr and PbI 2 Or the bulk CsPbBri 2 。
5. The method according to claim 1, wherein a perovskite raw material is additionally charged during the heat treatment.
6. The method of claim 5, wherein the perovskite starting material is CsPbBr in bulk phase 3 The mass ratio of the additional input amount of the perovskite raw material to the porous material is 1: (1-10).
7. The method according to claim 5, wherein the perovskite raw material is CsBr or PbI 2 Is additionally added into the perovskite raw material, csBr and PbI 2 The mass ratio of the porous material to the porous material is 1:2 (5-15).
8. The method of claim 1, wherein the poor solvent comprises an alcohol and/or toluene.
9. The method of claim 8, wherein the poor solvent is isopropyl alcohol.
10. The method according to claim 1, wherein the temperature of the heat treatment is 350 to 1000 ℃.
11. The method according to claim 1, wherein the heating treatment has a heating rate of 1 to 15 ℃/min.
12. The method according to claim 1, wherein the heat-treatment is carried out for a period of 10 to 180 minutes.
13. A reinforced core-shell anchored perovskite quantum dot, characterized in that the reinforced core-shell anchored perovskite quantum dot comprises an outer shell and a perovskite quantum dot core arranged in the outer shell, wherein the perovskite quantum dot core is anchored with the outer shell in a bonding way, and the reinforced core-shell anchored perovskite quantum dot is prepared by the preparation method of the reinforced core-shell anchored perovskite quantum dot according to any one of claims 1 to 12.
14. Use of the enhanced core-shell anchored perovskite quantum dot of claim 13, wherein said enhanced core-shell anchored perovskite quantum dot is used in an optoelectronic device.
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| CN114621749A (en) * | 2022-03-28 | 2022-06-14 | 无锡极电光能科技有限公司 | Preparation method of perovskite quantum dots |
| CN114656952B (en) * | 2022-03-29 | 2023-10-27 | 无锡极电光能科技有限公司 | Perovskite quantum dot and preparation method and application thereof |
| CN115433563A (en) * | 2022-09-01 | 2022-12-06 | 无锡极电光能科技有限公司 | Perovskite quantum dot with core-shell structure and preparation method and application thereof |
| CN115637149B (en) * | 2022-10-19 | 2024-04-05 | 无锡极电光能科技有限公司 | Perovskite quantum dot diffusion plate and preparation method thereof |
| CN116004228B (en) * | 2022-12-26 | 2024-04-26 | 无锡极电光能科技有限公司 | Surface modified perovskite quantum dot, preparation method thereof and core-shell structure quantum dot |
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