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CN113214830A - Double-acid assisted synthesis of CsPbX3Method for quantum dots - Google Patents

Double-acid assisted synthesis of CsPbX3Method for quantum dots Download PDF

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CN113214830A
CN113214830A CN202110500565.6A CN202110500565A CN113214830A CN 113214830 A CN113214830 A CN 113214830A CN 202110500565 A CN202110500565 A CN 202110500565A CN 113214830 A CN113214830 A CN 113214830A
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cspbx
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dodecylbenzenesulfonic
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宋继中
张百松
方涛
袁诗晨
杨林翔
李贤胜
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Nanjing University of Science and Technology
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Abstract

本发明公开了一种双酸辅助合成CsPbX3量子点的方法。所述方法采用两种具有不同空间位阻的有机酸来溶解铯盐形成铯前驱体，溴化铅和四正辛基溴化铵加入甲苯中形成铅前驱体，最后将铯前驱体注入到铅前驱体中，搅拌反应得到CsPbX3量子点。本发明采用双酸调控合成稳定的高质量CsPbX3量子点，其发光性能和结晶质量得到增强，可用于制备高发光效率的CsPbX3量子点发光器件。

Figure 202110500565

The invention discloses a method for synthesizing CsPbX 3 quantum dots assisted by diacids. The method uses two organic acids with different steric hindrances to dissolve cesium salts to form cesium precursors, lead bromide and tetra-n-octylammonium bromide are added to toluene to form lead precursors, and finally the cesium precursors are injected into lead. In the precursor, the stirring reaction gave CsPbX 3 quantum dots. The invention adopts diacid regulation to synthesize stable high-quality CsPbX 3 quantum dots, the luminescence performance and crystal quality are enhanced, and can be used for preparing high luminous efficiency CsPbX 3 quantum dot light-emitting devices.

Figure 202110500565

Description

Double-acid assisted synthesis of CsPbX3Method for quantum dots
Technical Field
The invention belongs to the technical field of quantum dot synthesis, and relates to a double-acid-assisted synthesis CsPbX3A method of quantum dots.
Background
CsPbX3The quantum dot material has the advantages of extremely high quantum yield, narrow light-emitting peak, high carrier mobility, high defect tolerance and the like, and has great development potential in the photoelectric fields of LED devices, solar cells, detectors and the like. However, CsPbX prepared by the existing method3The low luminous efficiency and colloid instability of the quantum dots limit further application thereof. CsPbI prepared from precursor of Xia et al using palmitic acid as solvent3Quantum dots have High PLQY (up to 92%), and palmitic acid can inhibit agglomeration of quantum dots, thereby reducing their regeneration-induced instability (Xia, H.; Wu, S.; Li, L.; Zhang, S., High binding affinity and controlled formation of CsPbX)3(X-Cl/Br, Br, I) peroxide nanocrystals with high quality standards and enhanced stability RSC adv.2018,8(63), 35973-. Yang et al use benzenesulfonic acid as a solvent precursor to prepare perovskite quantum dots, which can firmly bind non-coordinated lead ions and effectively eliminate exciton trapping probability caused by bromine vacancies (Yang, D.; Li, X.; Zhou, W.; et al, CsPbBr)3Quantum Dots 2.0 Benzenesulfonic Acid Equivalent liquid organic and Awakens Complete purification. adv. Mater.2019,31(30), e 1900767.). Tan et al prepared CsPbX from precursors containing octylphosphonic acid3Quantum dots, the quantum dots obtained, due to the strong interaction between Octylphosphonic Acid and lead atoms, obtained high quality dispersion in solvents after multiple purifications, the QLEDs prepared correspond to an external quantum efficiency of 6.5% (Tan, Y.; Zou, Y.; Wu, L.; et al., high luminescence and Stable Perovskite Nanocrystals with an octyl phosphonic Acid as a Light and for Efficient Light-Emitting diodes ACS. Appl. matrix. interfaces 2018,10(4), 3784-3792.). However, the CsPbX synthesized by using monoacid as a surface chelating ligand3The method of quantum dots still has the problem of loss of a large amount of ligands, so that poor colloidal stability is easily caused, and the light efficiency of the quantum dots and the dispersibility of the quantum dots in a solvent are greatly reduced. Therefore, it is urgentDevelopment of suitable acid ligands is required to efficiently passivate CsPbX3The surface defects of the quantum dots and the combination of the ligands and the quantum dots are enhanced, so that the colloidal stability and the luminous efficiency of the quantum dots are improved.
Disclosure of Invention
The invention aims to provide a double-acid-assisted synthesis CsPbX for effectively improving the stability and the luminous efficiency of quantum dot glue3A method of quantum dots.
The technical scheme for realizing the purpose of the invention is as follows:
double-acid assisted synthesis of CsPbX3A method of quantum dots comprising the steps of:
(1) dissolving cesium carbonate in a mixed solution of organic acids to form a cesium precursor, wherein the organic acids are two selected from n-octanoic acid, oleic acid, dodecylbenzene sulfonic acid and n-octylphosphoric acid;
(2) adding lead bromide and tetra-n-octyl ammonium bromide into toluene, and stirring and dissolving in air at room temperature to form a lead precursor;
(3) injecting a cesium precursor into a lead precursor, and stirring for reaction to obtain CsPbX3Adding the quantum dot stock solution into a purification solvent for centrifugation, and re-dispersing the centrifuged precipitate in an organic solvent to obtain purified CsPbX3And (4) quantum dots.
Preferably, in the step (1), the concentration of cesium carbonate in the cesium precursor is 0.2-1 mol/L.
Preferably, in the step (1), the mixed solution of the organic acid is a mixed solution of n-octanoic acid and oleic acid, a mixed solution of n-octanoic acid and dodecylbenzene sulfonic acid, a mixed solution of n-octanoic acid and n-octylphosphoric acid, a mixed solution of oleic acid and dodecylbenzene sulfonic acid, a mixed solution of oleic acid and n-octylphosphoric acid, or a mixed solution of dodecylbenzene sulfonic acid and n-octylphosphoric acid.
Preferably, in the mixed solution of the n-caprylic acid and the oleic acid, the volume ratio of the n-caprylic acid to the oleic acid is 4: 6-8: 2.
Preferably, in the mixed solution of the n-octanoic acid and the dodecylbenzene sulfonic acid, the volume ratio of the n-octanoic acid to the dodecylbenzene sulfonic acid is 3: 7-7: 3.
Preferably, in the mixed solution of n-octanoic acid and n-octylphosphoric acid, the volume ratio of n-octanoic acid to n-octylphosphoric acid is 3: 7-8: 2.
Preferably, in the mixed solution of oleic acid and dodecylbenzene sulfonic acid, the volume ratio of oleic acid to dodecylbenzene sulfonic acid is 2: 8-3: 7.
Preferably, in the mixed solution of oleic acid and n-octyl phosphoric acid, the volume ratio of oleic acid to n-octyl phosphoric acid is 3: 7-5: 5.
Preferably, in the mixed solution of dodecylbenzene sulfonic acid and n-octylphosphoric acid, the volume ratio of dodecylbenzene sulfonic acid to n-octylphosphoric acid is 3: 7-6: 4.
Preferably, in the step (2), the concentration of lead bromide in the lead precursor is 0.02-0.1 mol/L, and the concentration of tetra-n-octylammonium bromide is 0.04-0.2 mol/L.
Preferably, in the step (3), the stirring reaction time is 1-5 min.
Preferably, in the step (3), the purification solvent is a purification solvent conventionally used in the art, such as ethyl acetate, methyl acetate, butyl acetate, isopropanol, n-butanol, t-butanol, acetone, and the like; the CsPbX3The volume ratio of the quantum dot stock solution to the purification solvent is 1: 1-1: 3.
In the step (3), the organic solvent is conventionally used in the art for dispersing CsPbX3Organic solvents for quantum dots, such as n-hexane, n-octane, toluene, and the like.
Compared with the prior art, the invention has the following advantages:
the present invention utilizes two organic acids with different steric hindrance to dissolve cesium salt, and deprotonation functional group of organic acid can be reacted with CsPbX3The uncoordinated lead ions on the surface of the quantum dot are combined and simultaneously bonded with CsPbX through hydrogen bonds3And (3) bromine ion interaction on the surface of the quantum dot. Different steric hindrance of the double organic acids can further improve CsPbX3The surface state of the quantum dot leads the ligand to be orderly combined on the surface, and the exciton recombination is enhanced. The invention adopts the dual acid to regulate and synthesize the stable high-quality CsPbX3Quantum dots, synthesisCsPbX of3The quantum dots have nearly consistent quantum yield and high photoluminescence intensity, the luminescent performance and the crystallization quality of the quantum dots are enhanced, and the quantum dots can be used for preparing CsPbX with high luminescent efficiency3A quantum dot light emitting device.
Drawings
Fig. 1 is an XRD pattern of the quantum dot prepared in example 1.
Fig. 2 is PL plots corresponding to quantum dots obtained in comparative example, example 1, example 2, and example 3.
Fig. 3 is PL plots corresponding to the quantum dots obtained in comparative example, example 2, example 4, and example 5.
Fig. 4 is PL plots corresponding to the quantum dots obtained in comparative example, example 6, example 7, and example 8.
Fig. 5 is a graph of EQE for QLEDs prepared in comparative example, example 1, example 2, and example 3.
Fig. 6 is a graph of EQE for QLEDs prepared in comparative example, example 2, example 4, and example 5.
Fig. 7 is a graph of EQE for QLEDs prepared in comparative example, example 6, example 7, and example 8.
Detailed Description
The invention is described in more detail below with reference to specific embodiments and the accompanying drawings.
Example 1
1) Dissolving 2mmol of cesium carbonate in 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzene sulfonic acid, and stirring the solution in air at room temperature until the cesium carbonate is completely dissolved to prepare a cesium precursor;
2) adding 2mmol of lead bromide and 4.4mmol of tetra-n-octyl ammonium bromide into 30mL of toluene, and stirring the mixture in air at room temperature until the mixture is completely dissolved to obtain a lead precursor;
3) adding a cesium precursor into a lead precursor solution in a reaction flask, and reacting for 3min to obtain CsPbX3Adding 60mL of ethyl acetate into the quantum dot stock solution, centrifuging to remove supernatant, and dispersing the precipitate in 10mL of n-octane to obtain CsPbBr3Quantum dots;
4) sequentially spin-coating PEDOT, PSS, PTAA and CsPbBr on a glass substrate with an ITO electrode3Quantum dots ofAnd sequentially evaporating 40nm of TPBi, 1nm of LiF and 100nm of Al electrodes in the thermal evaporation cavity to obtain the QLED device.
Comparative example 1
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 5mL of n-octanoic acid, and the other conditions were kept the same.
Example 2
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 2.5mL of n-octanoic acid and 2.5mL of dodecylbenzenesulfonic acid, and the other conditions were kept the same.
Example 3
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 3.5mL of n-octanoic acid and 1.5mL of dodecylbenzenesulfonic acid, and the other conditions were kept the same.
Example 4
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 2.5mL of n-octanoic acid and 2.5mL of oleic acid, and the other conditions were kept the same.
Example 5
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 2.5mL of n-octanoic acid and 2.5mL of n-octylphosphoric acid, and the other conditions were kept the same.
Example 6
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 1mL of oleic acid and 4mL of dodecylbenzenesulfonic acid, and the other conditions were kept the same.
Example 7
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 2mL of oleic acid and 3mL of n-octylphosphoric acid, and the other conditions were kept the same.
Example 8
The same procedure as in example 1 was used except that 1.5mL of n-octanoic acid and 3.5mL of dodecylbenzenesulfonic acid in step 1) of example 1 were changed to 2.5mL of n-octylphosphoric acid and 2.5mL of dodecylbenzenesulfonic acid, and the other conditions were kept the same.
As can be seen from FIG. 1, the synthesis of CsPbX assisted by diacid3The nanocrystal is good in crystallinity. FIGS. 2, 3 and 4 show the synthesized CsPbX3The nanocrystalline has a narrow high-purity green light luminous peak (the half-peak width is less than 20nm, and the luminous peak is about 516 nm). As can be seen from FIGS. 5, 6 and 7, the room temperature quantum dots synthesized by the aid of the diacid can achieve a luminous efficiency of over 10 percent and a maximum of 17 percent even without further improvement, which is obviously higher than that of CsPbX synthesized by the monoacid3And (4) quantum dots.

Claims (10)

1.双酸辅助合成CsPbX3量子点的方法，其特征在于，包括如下步骤：1. the method for synthesizing CsPbX 3 quantum dots with the aid of diacid, is characterized in that, comprises the steps: (1)将碳酸铯溶解在有机酸的混合溶液中，形成铯前驱体，所述的有机酸选自正辛酸、油酸、十二烷基苯磺酸和正辛基磷酸中的两种；(1) cesium carbonate is dissolved in the mixed solution of organic acid, forms cesium precursor, and described organic acid is selected from two kinds in n-octanoic acid, oleic acid, dodecylbenzenesulfonic acid and n-octylphosphoric acid; (2)将溴化铅和四正辛基溴化铵加入甲苯中，在室温、空气中搅拌溶解，形成铅前驱体；(2) lead bromide and tetra-n-octylammonium bromide are added in toluene, stirring and dissolving in room temperature, air, form lead precursor; (3)将铯前驱体注入到铅前驱体中，搅拌反应得到CsPbX3量子点原液，再加入提纯溶剂离心，将离心后的沉淀再分散在有机溶剂中得到纯化的CsPbX3量子点。(3) Inject the cesium precursor into the lead precursor, stir and react to obtain the CsPbX 3 quantum dot stock solution, then add a purification solvent for centrifugation, and redisperse the centrifuged precipitate in an organic solvent to obtain purified CsPbX 3 quantum dots. 2.根据权利要求1所述的方法，其特征在于，步骤(1)中，所述的铯前驱体中，碳酸铯的浓度为0.2～1mol/L。2 . The method according to claim 1 , wherein, in the step (1), in the cesium precursor, the concentration of cesium carbonate is 0.2-1 mol/L. 3 . 3.根据权利要求1所述的方法，其特征在于，步骤(1)中，所述的有机酸的混合溶液为正辛酸和油酸的混合溶液，正辛酸和十二烷基苯磺酸的混合溶液，正辛酸和正辛基磷酸的混合溶液，油酸和十二烷基苯磺酸的混合溶液，油酸和正辛基磷酸的混合溶液，或十二烷基苯磺酸和正辛基磷酸的混合溶液。3. method according to claim 1, is characterized in that, in step (1), the mixed solution of described organic acid is the mixed solution of n-octanoic acid and oleic acid, the mixed solution of n-octanoic acid and dodecylbenzenesulfonic acid Mixed solution, mixed solution of n-octyl acid and n-octyl phosphoric acid, mixed solution of oleic acid and dodecylbenzenesulfonic acid, mixed solution of oleic acid and n-octylphosphoric acid, or mixed solution of dodecylbenzenesulfonic acid and n-octylphosphoric acid mixture. 4.根据权利要求1所述的方法，其特征在于，所述的正辛酸和油酸的混合溶液中，正辛酸与油酸的体积比为4:6～8:2；所述的正辛酸和十二烷基苯磺酸的混合溶液中，正辛酸和十二烷基苯磺酸的体积比为3:7～7:3。4. method according to claim 1, is characterized in that, in the mixed solution of described n-octanoic acid and oleic acid, the volume ratio of n-octanoic acid and oleic acid is 4:6～8:2; In the mixed solution with dodecylbenzenesulfonic acid, the volume ratio of n-octanoic acid and dodecylbenzenesulfonic acid is 3:7-7:3. 5.根据权利要求1所述的方法，其特征在于，所述的正辛酸和正辛基磷酸的混合溶液中，正辛酸和正辛基磷酸的体积比为3:7～8:2；所述的油酸和十二烷基苯磺酸的混合溶液中，油酸和十二烷基苯磺酸的体积比为2:8～3:7。5. method according to claim 1, is characterized in that, in the mixed solution of described n-octyl acid and n-octyl phosphoric acid, the volume ratio of n-octyl acid and n-octyl phosphoric acid is 3:7～8:2; In the mixed solution of oleic acid and dodecylbenzenesulfonic acid, the volume ratio of oleic acid and dodecylbenzenesulfonic acid is 2:8-3:7. 6.根据权利要求1所述的方法，其特征在于，所述的油酸和正辛基磷酸的混合溶液中，油酸和正辛基磷酸的体积比为3:7～5:5；所述的十二烷基苯磺酸和正辛基磷酸的混合溶液中，十二烷基苯磺酸和正辛基磷酸的体积比为3:7～6:4。6. method according to claim 1, is characterized in that, in the mixed solution of described oleic acid and n-octyl phosphoric acid, the volume ratio of oleic acid and n-octyl phosphoric acid is 3:7～5:5; In the mixed solution of dodecylbenzenesulfonic acid and n-octylphosphoric acid, the volume ratio of dodecylbenzenesulfonic acid and n-octylphosphoric acid is 3:7-6:4. 7.根据权利要求1所述的方法，其特征在于，步骤(2)中，所述的铅前驱体中，溴化铅的浓度为0.02～0.1mol/L，四正辛基溴化铵的浓度为0.04～0.2mol/L。7. method according to claim 1, is characterized in that, in step (2), in described lead precursor, the concentration of lead bromide is 0.02～0.1mol/L, and the concentration of tetra-n-octylammonium bromide is 0.02～0.1mol/L. The concentration is 0.04～0.2mol/L. 8.根据权利要求1所述的方法，其特征在于，步骤(3)中，所述的搅拌反应时间为1～5min。8. The method according to claim 1, characterized in that, in step (3), the stirring reaction time is 1-5 min. 9.根据权利要求1所述的方法，其特征在于，步骤(3)中，所述的提纯溶剂为乙酸乙酯、乙酸甲酯、乙酸丁酯、异丙醇、正丁醇、叔丁醇或丙酮；所述的CsPbX3量子点原液与提纯溶剂的体积比为1:1～1:3。9. method according to claim 1, is characterized in that, in step (3), described purifying solvent is ethyl acetate, methyl acetate, butyl acetate, isopropanol, n-butanol, tert-butanol or acetone; the volume ratio of the CsPbX 3 quantum dot stock solution to the purification solvent is 1:1 to 1:3. 10.根据权利要求1所述的方法，其特征在于，所述的有机溶剂为正己烷、正辛烷或甲苯。10. The method according to claim 1, wherein the organic solvent is n-hexane, n-octane or toluene.
CN202110500565.6A 2021-05-08 2021-05-08 Double-acid assisted synthesis of CsPbX3Method for quantum dots Pending CN113214830A (en)

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CN110157408A (en) * 2019-05-17 2019-08-23 南京理工大学 Method for Synthesizing Efficient and Stable All-Inorganic Halogen Perovskite Quantum Dot Scintillators with Equivalent Ligands
CN111081816A (en) * 2019-12-19 2020-04-28 华中科技大学 Perovskite nanocrystalline with alkali metal ion passivated surface defect and preparation and application thereof
CN111117598A (en) * 2019-12-19 2020-05-08 华中科技大学 ABX based on room temperature methodnY3-nLigand regulation method and application of perovskite nano particles
CN111171813A (en) * 2020-01-07 2020-05-19 鲁东大学 All-inorganic perovskite CsPbBr3Preparation method of quantum dot superlattice
CN111205853A (en) * 2020-01-22 2020-05-29 上海应用技术大学 A kind of preparation method of silica-coated all-inorganic perovskite core-shell quantum dots
CN111268724A (en) * 2020-02-14 2020-06-12 南京理工大学 Synthesis of CsPbI by room-temperature nonpolar solvent system3Method for perovskite nanocrystalline
CN112625680A (en) * 2020-12-29 2021-04-09 福州大学 Method for improving stability of mixed halogen perovskite

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