CN110746966A - Preparation method of perovskite quantum dot and perovskite quantum dot - Google Patents

Preparation method of perovskite quantum dot and perovskite quantum dot Download PDF

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CN110746966A
CN110746966A CN201910939121.5A CN201910939121A CN110746966A CN 110746966 A CN110746966 A CN 110746966A CN 201910939121 A CN201910939121 A CN 201910939121A CN 110746966 A CN110746966 A CN 110746966A
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perovskite
quantum dot
precursor
perovskite quantum
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CN110746966B (en
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翟伟
邢泽咏
刘思锦
王允军
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Suzhou Xingshuo Nanotech Co Ltd
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Abstract

The application discloses a preparation method of perovskite quantum dots, which comprises the following steps: s1, providing A4BX6Perovskite type; s2, making A4BX6Mixing perovskite with a precursor substance containing halogen, and reacting at a first temperature to obtain perovskite quantum dots, wherein the first temperature is 100-240 ℃. In the present application A4BX6The perovskite is used as a reaction precursor to prepare the perovskite quantum dot, the reaction controllability is strong, a product of a required emission peak position can be prepared easily, and particularly, the fluorescent emission peak of the perovskite quantum dot containing a single halogen species has a wider adjustment range. The perovskite quantum dot obtained by the preparation method has narrow half-peak width of an emission peak and excellent luminescence property, so that the application range of the perovskite quantum dot is expanded.

Description

Preparation method of perovskite quantum dot and perovskite quantum dot
Technical Field
The application relates to the field of nanotechnology, in particular to a preparation method of perovskite quantum dots and the perovskite quantum dots.
Background
Perovskite quantum dots are novel semiconductor nanoparticles, have the advantages of high luminous efficiency, simple synthesis conditions and the like, and are regarded as excellent luminescent materials and are paid attention by researchers.
When the perovskite quantum dots are prepared by the existing method, the product with the required luminescent property is obtained by adjusting the type, the adding amount, the reaction temperature, the reaction time and the like of reaction raw materials. However, the effect of the regulation and control method is not good, the reaction controllability in the regulation and control process is poor, the required perovskite quantum dots are difficult to obtain directly, and the optical performance of the perovskite quantum dots is to be improved, so that the application and use range of the perovskite quantum dots is limited.
Therefore, there is a need for an improvement of the existing methods for preparing perovskite quantum dots.
Disclosure of Invention
In view of the above technical problems, an object of the present application is to provide a method for preparing a perovskite quantum dot with good luminescence properties and controllable wavelength, and a perovskite quantum dot.
The application firstly provides a preparation method of perovskite quantum dots, which comprises the following steps:
s1, providing A4BX6Perovskite type;
s2, making A4BX6Mixing perovskite with a precursor substance containing halogen, and reacting at a first temperature to obtain the perovskite quantum dot, wherein the first temperature is 100-240 ℃.
Further, in said A4BX6In the perovskite, A is Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+B is Pb2+、Ge2+Or Sn2+At least one of (1), X is Cl-、Br-、I-At least one of (1).
Further, the halogen-containing precursor material is at least one of lead halide, tin halide and germanium halide.
Further, in S2, the amount of A is measured by mass4BX6The ratio of perovskite-type to halogen-containing precursor material is 1: (4-12).
Further, the reaction system of S2 further includes a solvent and/or a ligand.
Further, in S1, A is4BX6The perovskite is prepared by synthesizing A4BX6The perovskite type perovskite is obtained by mixing a first precursor and a second precursor required by perovskite type perovskite and reacting at a second temperature, wherein the second temperature is 80-200 ℃.
Further, the first precursor is formed by Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+With at least one of a carboxylic acid anion, a carbonic acid anion, or a halogen anion; the second precursor is composed of Pb2+、Ge2+Or Sn2+With at least one of a carboxylic acid anion, an oxygen ion, or a halogen anion; and, at least one of the first precursor and the second precursor comprises a halide anion.
Further, the ratio of the first precursor to the second precursor is (1-5) by mass: 1.
further, the preparation method also comprises the following steps:
and S3, coating a shell layer on the perovskite quantum dot.
The application also provides a perovskite quantum dot prepared by the preparation method of any one of the perovskite quantum dots.
Has the advantages that:
in the present application A4BX6The perovskite is used as a reaction precursor to prepare the perovskite quantum dot, the reaction controllability is strong, a product of a required emission peak position can be prepared easily, and particularly, the fluorescent emission peak of the perovskite quantum dot containing a single halogen species has a wider adjustment range.
The perovskite quantum dot obtained by the preparation method has narrow half-peak width of an emission peak and excellent luminescence property, so that the application range of the perovskite quantum dot is expanded.
Detailed Description
The technical solutions in the examples of the present application will be described in detail below with reference to the embodiments of the present application. It should be noted that the described embodiments are only some embodiments of the present application, and not all embodiments.
According to a preferred embodiment of the present application, there is provided a method for preparing a perovskite quantum dot, comprising the steps of:
s1, providing A4BX6Perovskite type;
s2, making A4BX6Mixing perovskite with a precursor substance containing halogen, and reacting at a first temperature to obtain perovskite quantum dots, wherein the first temperature is 100-240 ℃.
According to a preferred embodiment of the present application, the first temperature is 150 to 200 ℃.
In the prior art, when perovskite quantum dots are prepared, precursor substances such as Cs salt, lead halide and the like required for synthesizing the perovskite quantum dots are usually directly mixed and reacted, and the required product is obtained by adjusting the type and the addition amount of the precursor substances, the temperature, the speed, the time and the like of the reaction. The inventor finds that the existing preparation method needs to control the luminescent characteristics of the prepared perovskite quantum dot by adjusting various reaction conditions, such as emission peak position, emission peak half-peak width, fluorescence quantum yield and the like, the regulation and control means is complex and has poor controllability, and the high-quality perovskite quantum dot with the required emission peak position is difficult to directly obtain.
In the present application, the inventors have found that A is directly reacted4BX6The perovskite is used as a reaction precursor for preparing the perovskite quantum dot, and the light-emitting characteristic of the prepared perovskite quantum dot can be more easily regulated. In the reaction process, the A with different particle sizes can be directly selected4BX6The perovskite type participates in the reaction, so that the perovskite quantum dots with required emission peak positions can be more easily obtained. In addition, the application directly leads A to be carried out without controlling excessive reaction conditions4BX6The perovskite reacts with a precursor substance containing halogen, so that the perovskite quantum dot with good optical performance, especially narrow half-peak width of emission peak can be conveniently obtained.
In addition, the inventor also finds that the prior art has more limited requirements on the injection temperature, the injection rate and the like of precursor substances when preparing perovskite quantum dots, such as high temperature and rapid injection and mutual reaction of the precursor substances. The preparation method has no specific limitation on the condition of the precursor substance participating in the reaction process, has stronger reaction controllability, and has very important reference significance for large-scale preparation of high-quality perovskite quantum dots.
In this application, A4BX6The perovskite-type can be obtained commercially directly or by pre-preparation. When the perovskite quantum dots are prepared, the A is directly taken4BX6Perovskite type, make it mix and react with precursor material comprising halogen, get products.
In addition, in the present application, A4BX6The perovskite-type can also be prepared in the process of preparing the perovskite quantum dot. In step S1 of the present application, synthesis a is first performed4BX6Mixing and reacting precursors required by perovskite type to obtain freshly prepared A-containing4BX6The perovskite-type mixed solution is then subjected to step S2 of the present application to obtain perovskite quantum dots.
It should be added that, in the present application, after a great deal of experimental operations, combined with experimental phenomena and analysis of experimental results, the inventors found that the above-mentioned preparation method of perovskite quantum dots is significantly different from the existing technology of directly mixing precursor substances required for synthesizing perovskite quantum dots, such as Cs salt, lead halide, etc., and reacting at a predetermined temperature to obtain a product, and the resulting technical effects are not the same. Firstly, the application does not need to regulate and control excessive reaction conditions, and can directly select different A4BX6The perovskite type quantum dots are used for preparing the required perovskite quantum dots, and the mode can enable the particle size distribution of the prepared perovskite quantum dots to be more uniform and the half-peak width of an emission peak to be narrower. Furthermore, the above-mentioned preparation method of the present application can also be achieved by merely selecting a different size of a4BX6The required specific peak value can be obtained by single regulation mode such as perovskite type or regulating the addition amount of precursor material containing halogenThe perovskite quantum dot of (1). In particular, the preparation method has wider adjustment range for the fluorescence emission peak of the perovskite quantum dot containing a single halogen species. For example, the all-inorganic pure bromine perovskite quantum dot CsPbBr prepared by the traditional hot injection method3The fluorescence emission peak is generally 508-515 nm, and the application makes Cs4PbBr6All-inorganic pure bromine perovskite quantum dot CsPbBr prepared by taking perovskite type as reaction precursor3And the fluorescence emission peak can reach 506-525nm, so that the wavelength regulation range of the all-inorganic pure bromine perovskite quantum dot is widened.
According to a preferred embodiment of the present application, at A4BX6In the perovskite, A is Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+B is Pb2+、Ge2+Or Sn2+At least one of (1), X is Cl-、Br-、I-At least one of (1).
In some exemplary embodiments of the present application, a4BX6The perovskite comprises Cs4PbCl6、Rb4PbCl6、[(R1R2R3R4N)]4PbCl6、[(R1R2N＝C(R3)-NR4R5)]4PbCl6、Cs4GeCl6、Rb4GeCl6、[(R1R2R3R4N)]4GeCl6、[(R1R2N＝C(R3)-NR4R5)]4GeCl6、Cs4SnCl6、Rb4SnCl6、[(R1R2R3R4N)]4SnCl6、[(R1R2N＝C(R3)-NR4R5)]4SnCl6、Cs4PbBr6、Rb4PbBr6、[(R1R2R3R4N)]4PbBr6、[(R1R2N＝C(R3)-NR4R5)]4PbBr6、Cs4GeBr6、Rb4GeBr6、[(R1R2R3R4N)]4GeBr6、[(R1R2N＝C(R3)-NR4R5)]4GeBr6、Cs4SnBr6、Rb4SnBr6、[(R1R2R3R4N)]4SnBr6、[(R1R2N＝C(R3)-NR4R5)]4SnBr6、Cs4PbI6、Rb4PbI6、[(R1R2R3R4N)]4PbI6、[(R1R2N＝C(R3)-NR4R5)]4PbI6、Cs4GeI6、Rb4GeI6、[(R1R2R3R4N)]4GeI6、[(R1R2N＝C(R3)-NR4R5)]4GeI6、Cs4SnI6、Rb4SnI6、[(R1R2R3R4N)]4SnI6、[(R1R2N＝C(R3)-NR4R5)]4SnI6、Cs4PbBr3I3、Rb4PbBr3I3、Cs4PbCl3Br3、Rb4PbCl3Br3、[(R1R2R3R4N)]4PbBr3I3、[(R1R2R3R4N)]4PbCl3Br3、[(R1R2N＝C(R3)-NR4R5)]4PbBr3I3、[(R1R2N＝C(R3)-NR4R5)]4PbCl3Br3、Cs4SnBr3I3、Rb4SnBr3I3、Cs4SnCl3Br3、Rb4SnCl3Br3、[(R1R2R3R4N)]4SnBr3I3、[(R1R2R3R4N)]4SnCl3Br3、[(R1R2N＝C(R3)-NR4R5)]4SnBr3I3、[(R1R2N＝C(R3)-NR4R5)]4SnCl3Br3、Cs4GeBr3I3、Rb4GeBr3I3、Cs4GeCl3Br3、Rb4GeCl3Br3、[(R1R2R3R4N)]4GeBr3I3、[(R1R2R3R4N)]4GeCl3Br3、[(R1R2N＝C(R3)-NR4R5)]4GeBr3I3、[(R1R2N＝C(R3)-NR4R5)]4GeCl3Br3One kind of (1). However, the exemplary embodiments of the present application are not limited thereto.
In some exemplary embodiments of the present application, R1To R5Each independently selected from hydrogen, deuterium, -F, -Cl, -Br, -I, hydroxy, substituted or unsubstituted C1-C60Alkyl, substituted or unsubstituted C2-C60Alkenyl, substituted or unsubstituted C2-C60Alkynyl, substituted or unsubstituted C1-C60Alkoxy, substituted or unsubstituted C6-C60And (4) an aryl group.
According to a preferred embodiment of the present application, the halogen-containing precursor material is at least one of a lead halide, a tin halide, a germanium halide.
In some exemplary embodiments of the present application, the halogen-containing precursor material comprises PbCl2、PbI2、PbBr2、SnCl2、SnI2、SnBr2、GeCl2、GeI2、GeBr2One kind of (1). However, the exemplary embodiments of the present application are not limited thereto.
According to a preferred embodiment of the present application, in S2, based on the amount of substance, a4BX6The ratio of perovskite-type to halogen-containing precursor material is 1: (4-12). The inventor finds that A4BX6The ratio of the amount of the perovskite to the amount of the halogen-containing precursor material is controlled within the above range, so that the obtained perovskite quantum dot has good fluorescence, and the perovskite quantum dot having good fluorescence emission characteristics can be prepared.
In the present application, the inventors have also found that A4BX6The ratio of the amount of the perovskite-type precursor material to the amount of the halogen-containing precursor material has a great influence on the structure of the prepared perovskite quantum dot.
In some exemplary embodiments of the present application, in S2, in terms of the amount of substance, a4BX6The ratio of perovskite-type to halogen-containing precursor species is in the range of 1: (4-8), and the ratio is not 1: 8. at the moment, the structure of the obtained perovskite quantum dot is a core-shell structure with gradient transition, wherein the core is A4BX6Perovskite of the type having a shell4BX6Perovskite quantum dots are generated by reaction of perovskite type and halogen-containing precursor materials.
In some exemplary embodiments of the present application, in S2, in terms of the amount of substance, a4BX6The ratio of perovskite-type to halogen-containing precursor species is in the range of 1: (8-12). At this time, the structure of the obtained perovskite quantum dot is a pure core structure, and the core structure is A4BX6Perovskite quantum dots are generated by reaction of perovskite type and halogen-containing precursor materials.
According to a preferred embodiment of the present application, the reaction system of S2 further comprises a solvent and/or a ligand.
According to a preferred embodiment of the present application, the solvent and/or the ligand comprises C6-C22Amine Compound, C6-C22Saturated or unsaturated amino acid, nitrogen-containing heterocyclic compound, C6-C40Saturated or unsaturated alkanes, C6-C30Aromatic hydrocarbons, C6-C22Phosphine oxide compound and C12-C22At least one aromatic ether. However, the exemplary embodiments of the present application are not limited thereto.
In some exemplary embodiments of the present application, the solvent and/or ligand is selected from C6-C22Primary alkylamines, e.g. hexadecylamine, C6-C22Secondary alkylamines, e.g. dioctylamine, C6-C40Tertiary alkyl amines, e.g. trioctylamine, nitrogen-containing heterocycles, e.g. pyridine, C6-C40Alkenes such as 1-octadecene, C6-C40Aliphatic hydrocarbons, e.g. hexadecane, octadecane, or squalane, with C6-C30Alkyl-substituted aromatic hydrocarbons, e.g. toluene, phenyldodecane, phenyltetradecane, or phenylhexadecane, substituted by C6-C22Alkyl-substituted phosphines, e.g. trioctylphosphine, substituted by C6-C22Alkyl-substituted phosphine oxides, e.g. trioctylphosphine oxide, C12-C22Aromatic ethers such as phenyl ether, or benzyl ether, myristic acid, palmitic acid, stearic acid, arachidic acid, oleic acid, tributylamine, tri-n-octylamine, oleylamine, or any combination thereof.
In the present application, the inventors found that adding the above-mentioned solvent and/or ligand during the synthesis of perovskite quantum dots can make a4BX6The perovskite type and the precursor material containing halogen react better and more fully, thereby being beneficial to the formation of the perovskite quantum dots and being beneficial to obtaining the perovskite quantum dots with higher quality and better optical performance.
According to a preferred embodiment of the present application, A4BX6The perovskite is prepared by synthesizing A4BX6Mixing a first precursor and a second precursor required for perovskite type formation, andobtained by reaction at a second temperature, wherein the second temperature is 80-200 ℃.
According to a preferred embodiment of the present application, the second temperature is 110 to 150 ℃.
In the present application, the inventors found that A is as described above4BX6The preparation method of the perovskite type perovskite is simple and feasible, the process is controllable, the reaction condition is mild, and A with different particle size ranges can be obtained by regulating and controlling the adding amount of the first precursor and the second precursor4BX6The perovskite is adopted, so that the perovskite quantum dots with required emission peak positions can be prepared subsequently.
According to a preferred embodiment of the present application, the first precursor is formed from Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+With at least one of a carboxylic acid anion, a carbonic acid anion, or a halogen anion.
In some exemplary embodiments of the present application, R1To R5Each independently selected from hydrogen, deuterium, -F, -Cl, -Br, -I, hydroxy, substituted or unsubstituted C1-C60Alkyl, substituted or unsubstituted C2-C60Alkenyl, substituted or unsubstituted C2-C60Alkynyl, substituted or unsubstituted C1-C60Alkoxy, substituted or unsubstituted C6-C60And (4) an aryl group.
In some exemplary embodiments of the present application, the first precursor is selected from one of cesium carboxylate, cesium carbonate, cesium halide, alkyl carboxylate amine, alkyl halide amine. However, the exemplary embodiments of the present application are not limited thereto. Further, the first precursor is selected from cesium oleate, CsCl, CsBr, CsI, Cs2CO3Rubidium oleate, RbCl, RbBr, RbI and Rb2CO3、CH3NH3Cl、CH3NH3Br、CH3NH3I、[HC(NH2)2]Cl、[HC(NH2)2]Br、[HC(NH2)2]In IOne of (1) and (b).
According to a preferred embodiment of the present application, the second precursor consists of Pb2+、Ge2+Or Sn2+With at least one of a carboxylic acid anion, an oxygen ion, or a halogen anion.
In some exemplary embodiments of the present application, the second precursor is selected from PbCl2、PbI2、PbBr2、GeCl2、GeI2、GeBr2、SnCl2、SnI2、SnBr2PbO, SnO and GeO. However, the exemplary embodiments of the present application are not limited thereto.
According to a preferred embodiment of the present application, at least one of the first precursor and the second precursor comprises a halide anion.
According to a preferred embodiment of the present application, the ratio of the first precursor to the second precursor is (1-5): 1. the inventors have found that controlling the ratio of the amounts of the first precursor to the second precursor in the above range allows a to be produced4BX6The perovskite has a stable structure and a good particle size distribution range, so that the subsequent preparation of the perovskite quantum dot with a narrow emission peak half-peak width is facilitated.
According to a preferred embodiment of the present application, the method for preparing perovskite quantum dots further comprises the steps of:
and S3, coating a shell layer on the perovskite quantum dot prepared in the S2.
According to a preferred embodiment of the present application, a precursor material required for synthesizing the shell layer of the perovskite quantum dot is added to the reaction system of S2, thereby coating the shell layer with the perovskite quantum dot. The inventor finds that the perovskite quantum dot coated with the shell layer is beneficial to obtaining the perovskite quantum dot with higher quantum efficiency, and the quantum dot has purer luminescence and narrow half-peak width.
In some exemplary embodiments of the present application, the precursor materials required to synthesize the shell of the perovskite quantum dot include at least a third precursor. Wherein the third precursor is made of Li+、Na+、K+、Rb+、Cs+、Fr+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+With at least one of a carboxylic acid anion, a carbonic acid anion, or a halogen anion. However, the exemplary embodiments of the present application are not limited thereto.
In some exemplary embodiments of the present application, R1To R5Each independently selected from hydrogen, deuterium, -F, -Cl, -Br, -I, hydroxy, substituted or unsubstituted C1-C60Alkyl, substituted or unsubstituted C2-C60Alkenyl, substituted or unsubstituted C2-C60Alkynyl, substituted or unsubstituted C1-C60Alkoxy, substituted or unsubstituted C6-C60And (4) an aryl group.
Further, the third precursor is selected from the group consisting of potassium carboxylate, sodium carboxylate, rubidium carboxylate, cesium carboxylate, alkylamine carboxylate, potassium carbonate, sodium carbonate, rubidium carbonate, cesium carbonate, potassium halide, sodium halide, rubidium halide, cesium halide, alkylamine halide, and the like. For example, the third precursor is selected from potassium oleate, sodium oleate, cesium oleate, rubidium oleate, KCl, NaCl, CsCl, RbCl, KBr, NaBr, CsBr, RbBr, KI, NaI, CsI, RbI, K2CO3、Na2CO3、Cs2CO3、RbCO3、CH3NH3Cl、CH3NH3Br、CH3NH3I、[CH(NH2)2]Cl、[CH(NH2)2]Br、[CH(NH2)2]I。
In some exemplary embodiments of the present application, the precursor material required for synthesizing the shell of the perovskite quantum dot further includes a fourth precursor. Wherein the fourth precursor is composed of Pb2+、Ge2+Or Sn2+With at least one of a carboxylic acid anion, an oxygen ion, or a halogen anion. However, the exemplary embodiments of the present application are not limited thereto. Further, the fourth precursor is selected from PbCl2、PbI2、PbBr2、GeCl2、GeI2、GeBr2、SnCl2、SnI2、SnBr2、PbO、SnO、GeO。
In some exemplary embodiments of the present application, the precursor material required for synthesizing the shell of the perovskite quantum dot may also be selected from mesoporous silica, siloxanes, alkyl phosphates, metal oxides, silicones, amine resins, molecular sieves, and the like. However, the exemplary embodiments of the present application are not limited thereto.
According to a preferred embodiment of the present application, the method for preparing perovskite quantum dots further comprises a step of purifying the obtained perovskite quantum dots to obtain high-purity perovskite quantum dots. These purification treatment steps are well known in the art and will not be described in detail here.
There is also provided, in accordance with a preferred embodiment of the present application, a perovskite quantum dot, which is produced by:
s1, providing A4BX6Perovskite type;
s2, making A4BX6Mixing perovskite with a precursor substance containing halogen, and reacting at a first temperature to obtain perovskite quantum dots, wherein the first temperature is 100-240 ℃.
According to a preferred embodiment of the present application, the first temperature is 150 to 200 ℃.
According to a preferred embodiment of the present application, at A4BX6In the perovskite, A is Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+B is Pb2+、Ge2+Or Sn2+At least one of (1), X is Cl-、Br-、I-At least one of (1).
In some exemplary embodiments of the present application, a4BX6The perovskite comprises Cs4PbCl6、Rb4PbCl6、[(R1R2R3R4N)]4PbCl6、[(R1R2N＝C(R3)-NR4R5)]4PbCl6、Cs4GeCl6、Rb4GeCl6、[(R1R2R3R4N)]4GeCl6、[(R1R2N＝C(R3)-NR4R5)]4GeCl6、Cs4SnCl6、Rb4SnCl6、[(R1R2R3R4N)]4SnCl6、[(R1R2N＝C(R3)-NR4R5)]4SnCl6、Cs4PbBr6、Rb4PbBr6、[(R1R2R3R4N)]4PbBr6、[(R1R2N＝C(R3)-NR4R5)]4PbBr6、Cs4GeBr6、Rb4GeBr6、[(R1R2R3R4N)]4GeBr6、[(R1R2N＝C(R3)-NR4R5)]4GeBr6、Cs4SnBr6、Rb4SnBr6、[(R1R2R3R4N)]4SnBr6、[(R1R2N＝C(R3)-NR4R5)]4SnBr6、Cs4PbI6、Rb4PbI6、[(R1R2R3R4N)]4PbI6、[(R1R2N＝C(R3)-NR4R5)]4PbI6、Cs4GeI6、Rb4GeI6、[(R1R2R3R4N)]4GeI6、[(R1R2N＝C(R3)-NR4R5)]4GeI6、Cs4SnI6、Rb4SnI6、[(R1R2R3R4N)]4SnI6、[(R1R2N＝C(R3)-NR4R5)]4SnI6、Cs4PbBr3I3、Rb4PbBr3I3、Cs4PbCl3Br3、Rb4PbCl3Br3、[(R1R2R3R4N)]4PbBr3I3、[(R1R2R3R4N)]4PbCl3Br3、[(R1R2N＝C(R3)-NR4R5)]4PbBr3I3、[(R1R2N＝C(R3)-NR4R5)]4PbCl3Br3、Cs4SnBr3I3、Rb4SnBr3I3、Cs4SnCl3Br3、Rb4SnCl3Br3、[(R1R2R3R4N)]4SnBr3I3、[(R1R2R3R4N)]4SnCl3Br3、[(R1R2N＝C(R3)-NR4R5)]4SnBr3I3、[(R1R2N＝C(R3)-NR4R5)]4SnCl3Br3、Cs4GeBr3I3、Rb4GeBr3I3、Cs4GeCl3Br3、Rb4GeCl3Br3、[(R1R2R3R4N)]4GeBr3I3、[(R1R2R3R4N)]4GeCl3Br3、[(R1R2N＝C(R3)-NR4R5)]4GeBr3I3、[(R1R2N＝C(R3)-NR4R5)]4GeCl3Br3One kind of (1). However, the exemplary embodiments of the present application are not limited thereto.
In some exemplary embodiments of the present application, R1To R5Each independently selected from hydrogen, deuterium, -F, -Cl, -Br, -I, hydroxy, substituted or unsubstituted C1-C60Alkyl, substituted or unsubstituted C2-C60Alkenyl, substituted or unsubstituted C2-C60Alkynyl, substituted or unsubstituted C1-C60Alkoxy, substituted or unsubstituted C6-C60And (4) an aryl group.
According to a preferred embodiment of the present application, the halogen-containing precursor material is at least one of a lead halide, a tin halide, a germanium halide.
In some exemplary embodiments of the present application, the halogen-containing precursor material comprises PbCl2、PbI2、PbBr2、SnCl2、SnI2、SnBr2、GeCl2、GeI2、GeBr2One kind of (1). However, the exemplary embodiments of the present application are not limited thereto.
According to a preferred embodiment of the present application, in S2, based on the amount of substance, a4BX6The ratio of perovskite-type to halogen-containing precursor material is 1: (4-12).
In some exemplary embodiments of the present application, in S2, in terms of the amount of substance, a4BX6The ratio of perovskite-type to halogen-containing precursor species is in the range of 1: (4-8), and the ratio is not 1: 8. at the moment, the structure of the obtained perovskite quantum dot is a core-shell structure with gradient transition, wherein the core is A4BX6Perovskite of the type having a shell4BX6Perovskite quantum dots are generated by reaction of perovskite type and halogen-containing precursor materials.
In some exemplary embodiments of the present application, in S2, in terms of the amount of substance, a4BX6The ratio of perovskite-type to halogen-containing precursor species is in the range of 1: (8-12). At this time, the result isThe obtained perovskite quantum dot has a pure core structure, and the core structure is A4BX6Perovskite quantum dots are generated by reaction of perovskite type and halogen-containing precursor materials.
According to a preferred embodiment of the present application, the reaction system of S2 further comprises a solvent and/or a ligand.
According to a preferred embodiment of the present application, the solvent and/or the ligand comprises C6-C22Amine Compound, C6-C22Saturated or unsaturated amino acid, nitrogen-containing heterocyclic compound, C6-C40Saturated or unsaturated alkanes, C6-C30Aromatic hydrocarbons, C6-C22Phosphine oxide compound and C12-C22At least one aromatic ether. However, the exemplary embodiments of the present application are not limited thereto.
In some exemplary embodiments of the present application, the solvent and/or ligand is selected from C6-C22Primary alkylamines, e.g. hexadecylamine, C6-C22Secondary alkylamines, e.g. dioctylamine, C6-C40Tertiary alkyl amines, e.g. trioctylamine, nitrogen-containing heterocycles, e.g. pyridine, C6-C40Alkenes such as 1-octadecene, C6-C40Aliphatic hydrocarbons, e.g. hexadecane, octadecane, or squalane, with C6-C30Alkyl-substituted aromatic hydrocarbons, e.g. toluene, phenyldodecane, phenyltetradecane, or phenylhexadecane, substituted by C6-C22Alkyl-substituted phosphines, e.g. trioctylphosphine, substituted by C6-C22Alkyl-substituted phosphine oxides, e.g. trioctylphosphine oxide, C12-C22Aromatic ethers such as phenyl ether, or benzyl ether, myristic acid, palmitic acid, stearic acid, arachidic acid, oleic acid, tributylamine, tri-n-octylamine, oleylamine, or any combination thereof.
According to a preferred embodiment of the present application, A4BX6The perovskite is prepared by synthesizing A4BX6The perovskite type perovskite is obtained by mixing a first precursor and a second precursor required by perovskite type perovskite and reacting at a second temperature, wherein the second temperature is 80-200 ℃.
According to a preferred embodiment of the present application, the second temperature is 110 to 150 ℃.
According to a preferred embodiment of the present application, the first precursor is formed from Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+With at least one of a carboxylic acid anion, a carbonic acid anion, or a halogen anion.
In some exemplary embodiments of the present application, R1To R5Each independently selected from hydrogen, deuterium, -F, -Cl, -Br, -I, hydroxy, substituted or unsubstituted C1-C60Alkyl, substituted or unsubstituted C2-C60Alkenyl, substituted or unsubstituted C2-C60Alkynyl, substituted or unsubstituted C1-C60Alkoxy, substituted or unsubstituted C6-C60And (4) an aryl group.
In some exemplary embodiments of the present application, the first precursor is selected from one of cesium carboxylate, cesium carbonate, cesium halide, alkyl carboxylate amine, alkyl halide amine. However, the exemplary embodiments of the present application are not limited thereto. Further, the first precursor is selected from cesium oleate, CsCl, CsBr, CsI, Cs2CO3Rubidium oleate, RbCl, RbBr, RbI and Rb2CO3、CH3NH3Cl、CH3NH3Br、CH3NH3I、[HC(NH2)2]Cl、[HC(NH2)2]Br、[HC(NH2)2]And (I) one of the compositions.
According to a preferred embodiment of the present application, the second precursor consists of Pb2+、Ge2+Or Sn2+With at least one of a carboxylic acid anion, an oxygen ion, or a halogen anion.
In some exemplary embodiments of the present application, the second precursor is selected from PbCl2、PbI2、PbBr2、GeCl2、GeI2、GeBr2、SnCl2、SnI2、SnBr2PbO, SnO and GeO. However, the exemplary embodiments of the present application are not limited thereto.
According to a preferred embodiment of the present application, at least one of the first precursor and the second precursor comprises a halide anion.
According to a preferred embodiment of the present application, the ratio of the first precursor to the second precursor is (1-5): 1.
according to a preferred embodiment of the present application, the perovskite quantum dots are prepared by:
s1, providing A4BX6Perovskite type;
s2, making A4BX6Mixing perovskite with a precursor substance containing halogen, and reacting at a first temperature to obtain perovskite quantum dots, wherein the first temperature is 100-240 ℃;
and S3, coating a shell layer on the perovskite quantum dot prepared in the S2.
According to a preferred embodiment of the present application, a precursor material required for synthesizing the shell layer of the perovskite quantum dot is added to the reaction system of S2, thereby coating the shell layer with the perovskite quantum dot.
In some exemplary embodiments of the present application, the precursor materials required to synthesize the shell of the perovskite quantum dot include at least a third precursor. Wherein the third precursor is made of Li+、Na+、K+、Rb+、Cs+、Fr+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+With at least one of a carboxylic acid anion, a carbonic acid anion, or a halogen anion. However, the exemplary embodiments of the present application are not limited thereto.
In some exemplary embodiments of the present application, R1To R5Each independently selected from hydrogen, deuterium, -F, -Cl, -Br, -I, hydroxy, substituted or unsubstituted C1-C60Alkyl, substituted or unsubstituted C2-C60Alkenyl, substituted or unsubstituted C2-C60Alkynyl, substituted or unsubstituted C1-C60Alkoxy, substituted or unsubstituted C6-C60And (4) an aryl group.
Further, the third precursor is selected from the group consisting of potassium carboxylate, sodium carboxylate, rubidium carboxylate, cesium carboxylate, alkylamine carboxylate, potassium carbonate, sodium carbonate, rubidium carbonate, cesium carbonate, potassium halide, sodium halide, rubidium halide, cesium halide, alkylamine halide, and the like. For example, the third precursor is selected from potassium oleate, sodium oleate, cesium oleate, rubidium oleate, KCl, NaCl, CsCl, RbCl, KBr, NaBr, CsBr, RbBr, KI, NaI, CsI, RbI, K2CO3、Na2CO3、Cs2CO3、RbCO3、CH3NH3Cl、CH3NH3Br、CH3NH3I、[CH(NH2)2]Cl、[CH(NH2)2]Br、[CH(NH2)2]I。
In some exemplary embodiments of the present application, the precursor material required for synthesizing the shell of the perovskite quantum dot further includes a fourth precursor. Wherein the fourth precursor is composed of Pb2+、Ge2+Or Sn2+With at least one of a carboxylic acid anion, an oxygen ion, or a halogen anion. However, the exemplary embodiments of the present application are not limited thereto. Further, the fourth precursor is selected from PbCl2、PbI2、PbBr2、GeCl2、GeI2、GeBr2、SnCl2、SnI2、SnBr2、PbO、SnO、GeO。
In some exemplary embodiments of the present application, the precursor material required for synthesizing the shell of the perovskite quantum dot may also be selected from mesoporous silica, siloxanes, alkyl phosphates, metal oxides, silicones, amine resins, molecular sieves, and the like. However, the exemplary embodiments of the present application are not limited thereto.
The perovskite quantum dot has the advantages of adjustable fluorescence emission wavelength, narrow emission peak half-peak width and excellent luminescence property.
A method for preparing perovskite quantum dots according to some exemplary embodiments of the present application will be described in more detail below with reference to examples; however, the exemplary embodiments of the present application are not limited thereto.
Example 1
Perovskite quantum dot CsPbBr3The preparation method comprises the following steps:
s1, obtaining Cs4PbBr6Perovskite type;
s2, adding 0.16mmol Cs4PbBr6Perovskite type, 1.6mmol PbBr210mL of oleic acid, 15mL of oleylamine and 80mL of 1-octadecene are mixed and stirred, and react for 5min at 180 ℃ to obtain a solution containing perovskite quantum dots;
s3, purifying to obtain the perovskite quantum dot CsPbBr3。
And (3) testing and characterizing:
and (4) at room temperature, taking the perovskite quantum dot obtained in the step S3, testing the fluorescence absorption and emission spectrum of the perovskite quantum dot, determining that the luminescence wavelength is 520nm, the half-peak width is 17nm, and measuring that the fluorescence quantum efficiency is 64%.
Example 2
Perovskite quantum dot CsPbBr3The preparation method comprises the following steps:
s1, obtaining Cs-containing4PbBr6Solution of perovskite type:
s1-1, mixing 8mmol of Cs2CO3Mixing 10mL of oleic acid and 40mL of 1-octadecene, stirring, and heating until a clear and transparent solution is obtained to obtain a first mixed solution;
s1-2, adding 2mmol of PbBr2Mixing 7mL of oleic acid, 14mL of oleylamine and 80mL of 1-octadecene, stirring, and heating until a clear and transparent solution is obtained to obtain a second mixed solution;
s1-3, adding 15mL of the first mixed solution obtained in the step S1-1 into the second mixed solution obtained in the step S1-2, and reacting at 120 ℃ for 30min to obtain the Cs-containing substance4PbBr6A solution of a perovskite-type;
s2, adding 2mmol of PbBr27mL of oleic acid, 14mL of oleylamine and 60mL of 1-octadecene were mixed and stirred, and heated until a clear and transparent solution was obtained, obtaining a solution containing PbBr2The solution of (1);
s3, obtaining Cs by 16mL of S1-34PbBr6The solution of perovskite type is added to S2 containing PbBr2Reacting at 190 deg.C for 5min, purifying to obtain perovskite quantum dot CsPbBr3。
And (3) testing and characterizing:
and (4) at room temperature, taking the perovskite quantum dot obtained in the step S3, testing the fluorescence absorption and emission spectrum of the perovskite quantum dot, determining that the luminescence wavelength is 522nm, the half-peak width is 16nm, and testing that the fluorescence quantum efficiency is 61%.
Comparative example
Perovskite quantum dot CsPbBr3The preparation method comprises the following steps:
s1, adding 1.25mmol Cs2CO3Mixing 3mL of oleic acid and 20mL of 1-octadecene, stirring, and heating until a clear and transparent solution is obtained to obtain a first mixed solution;
s2, 1.6mmol of PbBr2Mixing 10mL of oleic acid, 15mL of oleylamine and 80mL of 1-octadecene, stirring, and heating until a clear and transparent solution is obtained to obtain a second mixed solution;
s3, adding 4mL of the first mixed solution obtained in the step S1 into the second mixed solution obtained in the step S2, and reacting at 180 ℃ for 5min to obtain a solution containing perovskite quantum dots;
s4, purifying to obtain the perovskite quantum dot CsPbBr3。
And (3) testing and characterizing:
and (4) at room temperature, taking the perovskite quantum dot obtained in the step S4, testing the fluorescence absorption and emission spectrum of the perovskite quantum dot, determining that the luminescence wavelength is 512nm, the half-peak width is 21nm, and testing that the fluorescence quantum efficiency is 55%.
As can be seen from the above examples and comparative examples, Cs is used herein4PbBr6Perovskite type serving as reaction precursor for preparing perovskite quantum dot CsPbBr3The reaction controllability is strong, the product with the fluorescence emission peak above 520nm can be easily prepared, and the perovskite quantum dot (CsPbBr) containing single halogen species is widened3) The wavelength control range of (1). In addition, the application also obtains the perovskite with narrower half-peak width of the emission peakAnd (4) mineral quantum dots.
Although the present disclosure has been described and illustrated in greater detail by the inventors, it should be understood that modifications and/or alterations to the above-described embodiments, or equivalent substitutions, will be apparent to those skilled in the art without departing from the spirit of the disclosure, and that no limitations to the present disclosure are intended or should be inferred therefrom.

Claims (10)

1. The preparation method of the perovskite quantum dot is characterized by comprising the following steps:
s1, providing A4BX6Perovskite type;
s2, making A4BX6Mixing perovskite with a precursor substance containing halogen, and reacting at a first temperature to obtain the perovskite quantum dot, wherein the first temperature is 100-240 ℃.
2. The method for producing a perovskite quantum dot as claimed in claim 1, wherein A is4BX6In the perovskite, A is Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+B is Pb2+、Ge2+Or Sn2 +At least one of (1), X is Cl-、Br-、I-At least one of (1).
3. The method according to claim 1, wherein the halogen-containing precursor material is at least one of a lead halide, a tin halide, and a germanium halide.
4. The method for producing a perovskite quantum dot as claimed in claim 1, wherein in S2, a is measured by mass4BX6Perovskite and said halogenThe ratio of precursor substances of the elements is 1: (4-12).
5. The method for preparing perovskite quantum dots according to claim 1, wherein the reaction system of S2 further comprises a solvent and/or a ligand.
6. The method for producing a perovskite quantum dot as claimed in claim 1, wherein in S1, a is4BX6The perovskite is prepared by synthesizing A4BX6The perovskite type perovskite is obtained by mixing a first precursor and a second precursor required by perovskite type perovskite and reacting at a second temperature, wherein the second temperature is 80-200 ℃.
7. The method of preparing a perovskite quantum dot as claimed in claim 6, wherein the first precursor is made of Cs+、Rb+、(R1R2R3R4N)+Or (R)1R2N＝C(R3)-NR4R5)+With at least one of a carboxylic acid anion, a carbonic acid anion, or a halogen anion; the second precursor is composed of Pb2+、Ge2+Or Sn2+With at least one of a carboxylic acid anion, an oxygen ion, or a halogen anion; and, at least one of the first precursor and the second precursor comprises a halide anion.
8. The method for producing a perovskite quantum dot as claimed in claim 6, wherein the ratio of the first precursor to the second precursor is (1 to 5): 1.
9. the method for preparing a perovskite quantum dot as claimed in claim 1, further comprising the steps of:
and S3, coating a shell layer on the perovskite quantum dot.
10. A perovskite quantum dot, characterized by being produced by the production method of a perovskite quantum dot as claimed in any one of claims 1 to 9.
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CN112986199A (en) * 2021-02-22 2021-06-18 江南大学 Fluorescence detection method for acid value in oil

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CN112986199A (en) * 2021-02-22 2021-06-18 江南大学 Fluorescence detection method for acid value in oil

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