An orange-red light-emitting nanocrystal based on fluid conduit reaction and a preparation method thereof

CN118853159BActive Publication Date: 2026-09-25SHANGHAI INST OF TECH
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Patent Information

Application Number
CN202410859506.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-06-28
Publication Date
2026-09-25
Estimated Expiration
2044-06-28

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Technical Problem

但该专利所提出的有机-无机杂化三线态上转换发光材料的制备过程繁琐复杂、增加了纳米晶发光特性不可再现性的可能

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[0037](1)本发明在亚毫米通道/反应器的流体中操纵,操作简单、高传热传质、节省时间,有限的小尺寸能够精确控制反应参数,从而克服批量处理固有的不可再现性和不连续性;

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Abstract

The application relates to an orange-red light-emitting nanocrystal based on a fluid pipeline reaction and a preparation method thereof, wherein the nanocrystal is a divalent manganese ion and trivalent lanthanum ion co-doped nanocrystal synthesized by mixing and reacting a cesium oleate precursor solution and a lead source-manganese source-lanthanum source precursor solution through a fluid pipeline system, the molar ratio of the lead source, the manganese source and the lanthanum source is 1:1:(0.1-1); the fluid pipeline system comprises a preparation zone pipeline, a T-shaped joint and a reaction zone pipeline, the cesium oleate precursor solution and the lead source-manganese source-lanthanum source precursor solution flow into the preparation zone pipeline in sequence, are mixed through the T-shaped joint and synthesize the nanocrystal through the reaction zone pipeline. Compared with the prior art, the halide perovskite nanocrystal prepared by the application has high light-emitting intensity and excellent stability.
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Description

Technical Field

[0001] This invention belongs to the field of materials preparation technology, and relates to an orange-red light-emitting nanocrystal based on fluid channel reaction and its preparation method. Background Technology

[0002] All-inorganic lead halide perovskite nanocrystals (NCs) CsPbX3 (X = Cl, Br, and I) have become an attractive class of materials for optoelectronic applications due to their excellent optical properties (e.g., compositionally tunable emission covering the entire visible spectrum, high photoluminescence quantum yield (PLQY), and low cost). Studies have found that ion doping can bring about rich optical properties and improved optoelectronic performance; for example, divalent manganese ions (Mn) from transition metals can be used to dopants. 2+ ), Mn 2+ Introducing new optical properties into perovskite NCs (such as CsPbCl3) can achieve new optical properties, showing that CsPbCl3 NCs exhibit narrow purple exciton emission and stable broad orange emission. 4 T1– 6 A1 Mn 2+ (dd transition).

[0003] But with Mn 2+ Compared to doped II–VI quantum dots, from CsPbCl3 NCs bulk to Mn 2+ The energy transfer efficiency is several orders of magnitude lower. Increasing the Mn content in the perovskite NCs matrix... 2+ High doping concentration is a common method to improve energy transfer efficiency. However, high doping concentrations introduce manganese-manganese (Mn-Mn) dimers and trapped states, leading to the formation of nonradiative recombination NCs centers and causing concentration quenching. Therefore, increasing the doping concentration from the perovskite host to Mn... 2+ Energy transfer efficiency while maintaining low Mn 2+ Doping enhances Mn 2+ The launch intensity is an issue that urgently needs to be addressed.

[0004] Patent CN115029134A discloses a method for preparing high-efficiency manganese (Mn)-doped CsPbCl3 nanocrystals using aluminum chloride as an auxiliary agent. The method involves adding cesium carbonate and oleic acid to 1-octadecene to obtain a cesium oleate precursor solution. Different amounts of auxiliary dopants—aluminum chloride, manganese chloride, lead chloride, tri-n-octylphosphine, oleic acid, and oleylamine—are added to the 1-octadecene. The mixture is heated under vacuum, then heated under a protective gas atmosphere, and finally mixed with the cesium carbonate precursor solution to react and obtain Mn-doped CsPbCl3 nanocrystals with different optical properties. However, the aluminum chloride-assisted preparation of Mn-doped CsPbCl3 nanocrystals in this patent only improves their luminescence efficiency, without further improving the stability of the Mn-doped CsPbCl3 nanocrystals.

[0005] Patent CN110564415A discloses a method for synergistically enhancing the ultraviolet radiation stability and optical properties of Mn:CsPbCl3 nanocrystals. This method includes: preparing a cesium precursor solution; preparing a tin (Sn) precursor; mixing the tin Sn precursor, octadecene, oleic acid, oleylamine, trioctylphosphine, lead chloride, and manganese chloride; forming Sn and Mn co-doped CsPbCl3 nanocrystals; and obtaining a Sn and Mn co-doped CsPbCl3 nanocrystal solution. However, in the Sn and Mn co-doped CsPbCl3 nanocrystals proposed in this patent, divalent tin ions (Sn...)... 2+ It is easily oxidized to tetravalent tin ions (Sn). 4+ ), leaving unnecessary divalent Sn vacancies, which serve as non-radiative recombination centers and quench emission.

[0006] Patent CN117025222A discloses an organic-inorganic hybrid triplet upconversion luminescent material based on composite nanocrystals, its preparation method, and its applications. The organic-inorganic hybrid triplet upconversion luminescent material is mainly prepared by dissolving composite nanocrystals in organic acceptors and organic luminescent molecules. The composite nanocrystals are prepared from rare earth halides and ionic nanocrystals. The method includes the preparation of a solution of oleic acid ligand-encapsulated lead halide and cerium halide octadecene precursors, the preparation of composite nanocrystals by thermal injection, and the preparation of a composite solution of composite nanocrystals with organic acceptors and organic luminescent molecules, ultimately yielding the organic-inorganic hybrid triplet upconversion luminescent material. However, the preparation process of the organic-inorganic hybrid triplet upconversion luminescent material proposed in this patent is cumbersome and complex, increasing the possibility of non-reproducible luminescent properties of the nanocrystals. Summary of the Invention

[0007] The purpose of this invention is to overcome at least one defect of the prior art and provide an orange-red light-emitting nanocrystal based on fluid channel reaction and its preparation method. The halide perovskite nanocrystals prepared by this invention have high luminescence intensity and excellent stability.

[0008] The objective of this invention can be achieved through the following technical solutions:

[0009] One of the technical solutions of this invention is to provide an orange-red light-emitting nanocrystal based on a fluid-channel reaction. This nanocrystal is a divalent manganese ion (Mn) synthesized by mixing and reacting a cesium oleate precursor solution and a lead-manganese-lanthanum source precursor solution through a fluid-channel system. 2+ ) and trivalent lanthanum ion (La 3+ The nanocrystals are co-doped with lead, manganese and lanthanum sources in a molar ratio of 1:1:(0.1-1).

[0010] The fluid piping system includes a preparation zone piping, a T-junction, and a reaction zone piping. The cesium oleate precursor solution and the lead-manganese-lanthanum source precursor solution flow into the preparation zone piping, are mixed through the T-junction, and are synthesized into nanocrystals through the reaction zone piping, respectively.

[0011] Generally speaking, except for divalent tin ions (Sn 2+ ), calcium ions (Ca 2+ ), zinc ions (Zn) 2+ ) and copper ions (Cu 2+ Besides, trivalent lanthanide metal ions are often used as dopants in the preparation of halide perovskite nanocrystals (NCs). 3+ Due to its affinity for divalent lead ions (Pb) 2+ With similar ionic radii, it is easier to incorporate CsPbCl3 NCs and replace Pb. 2+ Positioning to improve the photoelectric properties of perovskite NCs.

[0012] In addition, in order to address the difficulty of achieving Mn using existing technologies 2+ and La 3+ To address the challenges of continuous industrial production of co-doped CsPbCl3 perovskite NCs, this invention provides a novel, previously unreported method for the continuous industrial production of Mn based on fluid conduit reactions. 2+ and La 3+ A method for preparing CsPbCl3 co-doped perovskite NCs. Mn is achieved through a fluid-channel reaction technique. 2+ and La 3+ Co-doping was performed, and different La2+ concentrations were obtained by adjusting the ratio of lead chloride, manganese chloride, and lanthanum chloride. 3+ Doping amount on CsPbCl3:Mn 2+ The influence of NCs luminescence provides a new experimental technical route for the preparation of perovskite NCs.

[0013] Furthermore, the inner diameter of the preparation area pipe is 700-900μm, the outer diameter is 1400-1800μm, and the length is 500-2000mm;

[0014] The inner diameter of the reaction zone pipe is 700-900μm, the outer diameter is 1400-1800μm, and the length is 200-300mm.

[0015] As a preferred technical solution, the materials of the preparation zone pipeline and the reaction zone pipeline are perfluoroethylene propylene (FEP) or polytetrafluoroethylene (PTFE).

[0016] As a preferred technical solution, the fluid pipeline system includes an injection pump, through which the cesium oleate precursor solution and the lead-manganese-lanthanum source precursor solution are pumped into the flow channel.

[0017] As a preferred technical solution, the fluid pipeline system includes a heater, and the reaction zone is disposed on the heater, the heater increasing the temperature of the reaction zone.

[0018] One of the technical solutions of the present invention is to provide a method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction, the method comprising the following steps:

[0019] S1. Mix cesium source, oleic acid (OA) and octadecene (ODE), heat under an inert gas atmosphere, and wait for the solution to become clear to obtain cesium oleate precursor solution;

[0020] S2. Mix lead source, manganese source, lanthanum source, tri-n-octylphosphine (TOP) and octadecene, heat under an inert gas atmosphere, add oleic acid and oleylamine (OAm) as stabilizers and surfactants, continue heating under an inert gas atmosphere until dissolved, to obtain lead source-manganese source-lanthanum source precursor solution;

[0021] S3. The cesium oleate precursor solution and the lead-manganese-lanthanum source precursor solution are mixed and reacted through a fluid pipeline system to obtain orange-red light-emitting nanocrystals based on fluid pipeline reaction.

[0022] Furthermore, the cesium source in step S1 includes cesium carbonate (Cs2CO3) or cesium acetate (CsOAc).

[0023] Furthermore, in step S1, the molar / volume ratio of cesium source, oleic acid and octadecene is (1-5 mol):(1-5 L):(20-60 L).

[0024] Furthermore, in step S2, lead chloride (PbCl2) is used as the lead source, manganese chloride (MnCl2) is used as the manganese source, and lanthanum chloride (LaCl3) is used as the lanthanum source.

[0025] As a preferred technical solution, in step S2, lead acetate (Pb(OAc)2) can be used as the lead source, manganese acetate (Mn(OAc)2) can be used as the manganese source, and lanthanum acetate (La(OAc)3) can be used as the lanthanum source. In this case, chloride ions with the corresponding hydrochloride ratio need to be added.

[0026] Furthermore, in step S2, the molar / volume ratio of lead source, manganese source, tri-n-octylphosphine, octadecene, oleic acid and oleylamine is (0.1-0.4 mol):(0.1-0.4 mol):(1-4 L):(5-20 L):(1-2 L):(1-2 L).

[0027] As a preferred technical solution, the inert gas in steps S1 and S2 includes nitrogen or argon.

[0028] Furthermore, in step S1, the heating temperature is 100-140℃ and the time is 20-40 minutes.

[0029] Furthermore, the heating temperature in step S2 is 100-140℃, the heating time after the first mixing is 30-60 min, and the heating time after the second addition is 5-10 min.

[0030] Furthermore, the reaction temperature in step S3 is 170-210℃.

[0031] As a preferred technical solution, purification is performed after the reaction in step S3.

[0032] As a preferred technical solution, the purification process includes precipitation or centrifugation.

[0033] As a preferred technical solution, the centrifugation rate is 6000-12000 rpm and the time is 1-10 min.

[0034] As a preferred technical solution, the orange-red light-emitting nanocrystals based on fluid channel reaction are preserved in a solvent after purification.

[0035] As a preferred technical solution, the solvent includes n-hexane or toluene.

[0036] Compared with the prior art, the present invention has the following beneficial effects:

[0037] (1) The present invention is operated in the fluid of the submillimeter channel / reactor, which is simple to operate, has high heat and mass transfer, saves time, and the limited small size can accurately control the reaction parameters, thereby overcoming the inherent non-reproducibility and discontinuity of batch processing.

[0038] (2) The fluid pipeline reaction synthesis method used in this invention can achieve the synthesis of divalent manganese ions (Mn). 2+ ) and trivalent lanthanum ion (La 3+ The continuous large-scale preparation of co-doped halide perovskite (CsPbCl3) nanocrystals (NCs) enables the industrial production of CsPbCl3 NCs in the future, which has great application potential in the field of solid-state lighting.

[0039] (3) The Mn proposed in this invention 2+ and La 3+ Co-doping improves the CsPbCl3:Mn ratio. 2+ The luminescence intensity of the nanocrystals, along with the effective passivation of surface defects by excess halogen ions, further enhances the stability of NCs. Attached Figure Description

[0040] Figure 1The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction in the embodiments of the present invention and Comparative Example 1 are shown.

[0041] Figure 2 The X-ray diffraction (XRD) patterns of orange-red light-emitting nanocrystals based on fluid channel reaction in Embodiment 1 and Comparative Example 1 of the present invention are shown below.

[0042] Figure 3 The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction in Comparative Example 1 of this invention at different storage times;

[0043] Figure 4 The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction at different storage times in Embodiment 1 of the present invention;

[0044] Figure 5 The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction at different storage times in Embodiment 2 of the present invention;

[0045] Figure 6 The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction at different storage times in Embodiment 3 of the present invention;

[0046] Figure 7 The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction at different storage times in Example 4 of the present invention;

[0047] Figure 8 The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction at different storage times in Embodiment 5 of the present invention;

[0048] Figure 9 The photoluminescence spectra of orange-red light-emitting nanocrystals based on fluid channel reaction in Embodiment 1 and the comparative example of the present invention are shown. Detailed Implementation

[0049] The present invention will now be described in detail with reference to specific embodiments. These embodiments are based on the technical solution of the present invention and provide detailed implementation methods and specific operating procedures. However, the scope of protection of the present invention is not limited to the following embodiments.

[0050] Unless otherwise specified, the equipment used in the following embodiments is conventional equipment in the art; unless otherwise specified, the reagents used are commercially available products or prepared by conventional methods in the art. In the following embodiments, unless otherwise described in detail, conventional experimental methods in the art can be used.

[0051] Example 1:

[0052] An orange-red light-emitting nanocrystal based on fluid channel reaction and its preparation method are described below:

[0053] S1. Weigh 2.5 mmol of cesium carbonate (Cs2CO3), 2.5 mL of oleic acid (OA) and 40 mL of octadecene (ODE), heat to 120 °C under a nitrogen atmosphere, maintain for 30 min, and wait for the solution to become clear to obtain the cesium oleate precursor solution.

[0054] S2. Weigh 0.188 mmol lead chloride (PbCl2), 0.188 mmol manganese chloride (MnCl2), 0.038 mmol lanthanum chloride (LaCl3) (the molar ratio of PbCl2, MnCl2 and LaCl3 is 1:1:0.2), 2 mL tri-n-octylphosphine (TOP) and 10 mL ODE. Heat to 120 °C under a nitrogen atmosphere and maintain for 60 min. Add 1.2 mL OA and 1.2 mL oleylamine (OAm) and maintain for 10 min until the reagents in the beaker are dissolved to obtain a lead-manganese-lanthanum precursor solution.

[0055] S3. The cesium oleate precursor solution and the lead-manganese-lanthanum source precursor solution are pumped into a polytetrafluoroethylene (FEP) preparation zone pipeline with an inner diameter of 800 μm, an outer diameter of 1600 μm, and a length of 1000 mm using a precision injection pump. The precursor solutions are mixed through a T-junction and flow into the FEP reaction zone pipeline with an inner diameter of 800 μm, an outer diameter of 1600 μm, and a length of 250 mm. The oil bath temperature is controlled to be 190 °C to allow the lead halide perovskite (CsPbCl3) to react with divalent manganese ions (Mn) to react. 2+ Nanocrystals were synthesized in a pipeline to obtain Mn 2+ and La 3+ Co-doped CsPbCl3 nanocrystals were purified and preserved. Orange-red light-emitting nanocrystals based on fluid channel reaction were purified in hexane by centrifugation at 9000 rpm for 5 min.

[0056] Comparative Example 1:

[0057] An orange-red light-emitting nanocrystal based on fluid channel reaction and its preparation method are basically the same as in Example 1, except that LaCl3 is not added in step S2 to obtain Mn. 2+ Single-doped CsPbCl3 nanocrystals.

[0058] Example 2:

[0059] An orange-red light-emitting nanocrystal based on a fluid channel reaction and its preparation method are basically the same as in Example 1, except that the amount of LaCl3 added in step S2 is increased from 0.038 mmol to 0.075 mmol (the molar ratio of PbCl2, MnCl2 and LaCl3 is 1:1:0.4), to obtain Mn... 2+ and La 3+ Co-doped CsPbCl3 nanocrystals.

[0060] Example 3:

[0061] An orange-red light-emitting nanocrystal based on a fluid channel reaction and its preparation method are basically the same as in Example 1, except that the amount of LaCl3 added in step S2 is increased from 0.038 mmol to 0.113 mmol (the molar ratio of PbCl2, MnCl2 and LaCl3 is 1:1:0.6), to obtain MnCl3. 2+ and La 3+ Co-doped CsPbCl3 nanocrystals.

[0062] Example 4:

[0063] An orange-red light-emitting nanocrystal based on a fluid channel reaction and its preparation method are basically the same as in Example 1, except that the amount of LaCl3 added in step S2 is increased from 0.038 mmol to 0.150 mmol (the molar ratio of PbCl2, MnCl2 and LaCl3 is 1:1:0.8), to obtain MnCl3. 2+ and La 3+ Co-doped CsPbCl3 nanocrystals.

[0064] Example 5:

[0065] An orange-red light-emitting nanocrystal based on a fluid channel reaction and its preparation method are basically the same as in Example 1, except that the amount of LaCl3 added in step S2 is increased from 0.038 mmol to 0.188 mmol (the molar ratio of PbCl2, MnCl2 and LaCl3 is 1:1:1), to obtain Mn... 2+ and La 3+ Co-doped CsPbCl3 nanocrystals.

[0066] The emission spectra of the above nanocrystals were measured using a fluorescence spectrometer (HITACHI F-7000) at 365 nm.

[0067] like Figure 1 As shown, it can be seen that for Mn in Comparative Example 1 2+ In addition to exciton emission (~410 nm), doped CsPbCl3 nanocrystals also exhibited a broad emission band at ~600 nm, which originated from Mn.2+ : 4 T1→ 6 A1 transition, FWHM is ~90nm;

[0068] In the examples, trivalent lanthanum ions (La) 3+ The incorporation of ) significantly improved the CsPbCl3:Mn 2+ The luminescence intensity of nanocrystals, La in Example 4 3+ When the doping concentration reaches a molar ratio of PbCl2, MnCl2, and LaCl3 of 1:1:0.8, Mn... 2+ Mn has the highest luminescence intensity. 2+ The emission peak remains basically unchanged at ~600nm.

[0069] The above nanocrystals were tested using X-ray diffraction (XRD).

[0070] like Figure 2 As shown, the diffraction peaks in Example 1 and Comparative Example 1 are consistent with those in the standard card PDF#97-002-9072, indicating that Comparative Example 1 successfully prepared Mn. 2+ Mn-doped CsPbCl3 nanocrystals were successfully prepared in Example 1. 2+ and La 3+ Co-doped CsPbCl3 nanocrystals.

[0071] The above nanocrystals were placed in room temperature air environment, and their luminescence changes at 24h, 144h, 504h and 672h and 365nm were recorded.

[0072] Table 1 shows the stability of the nanocrystals in the examples and Comparative Example 1 after 672 hours.

[0073] Comparative Example 1 17.6% Example 1 71.8% Example 2 63.9% Example 3 90.0% Example 4 57.5% Example 5 92.6%

[0074] like Figures 3 to 8 As shown in Table 1, it can be seen that Mn in Comparative Example 1 2+ Single-doped CsPbCl3 nanocrystals showed Mn content after 672 hours of storage. 2+ The characteristic emission suffered severe loss, while Mn in Examples 1 to 5 2+ and La 3+ Mn content of co-doped CsPbCl3 nanocrystals at different storage times 2+ The feature emission loss is low, and in Example 5, Mn 2+ and La 3+ Co-doped CsPbCl3 nanocrystals showed Mn content after 672 hours of storage. 2+ The luminescence intensity can retain up to 92.6% of its original intensity, indicating that Mn 2+ and La 3+ Co-doping further improves Mn2+ Stability characteristics of doped CsPbCl3 nanocrystals.

[0075] Comparative Example 2:

[0076] An orange-red light-emitting nanocrystal based on fluid channel reaction and its preparation method are basically the same as in Example 1, except that in step S2, LaCl3 is added instead of aluminum chloride (AlCl3) to obtain Mn 2+ And Al 3+ Co-doped CsPbCl3 nanocrystals.

[0077] Comparative Example 3:

[0078] An orange-red light-emitting nanocrystal based on fluid channel reaction and its preparation method are basically the same as in Example 1, except that in step S2, LaCl3 is added instead of cerium chloride (CeCl3) to obtain Mn 2+ And Al 3+ Co-doped CsPbCl3 nanocrystals.

[0079] The preparation conditions for the above embodiments and comparative examples are shown in Table 2.

[0080] Table 2 shows the preparation conditions of nanocrystals in the examples and comparative examples.

[0081]

[0082] The emission spectra of the above nanocrystals were analyzed using a fluorescence spectrometer, and their spectral properties at 365 nm were tested.

[0083] like Figure 9 As shown in the figure, it can be seen that Al in Comparative Example 2 3+ The incorporation did not improve the CsPbCl3:Mn 2+ The luminescence intensity of nanocrystals;

[0084] Comparative Example 3 Ce 3+ The incorporation of [a specific ingredient] slightly increased the CsPbCl3:Mn [compound / component] ratio. 2+ The luminescence intensity of nanocrystals, but compared to Mn 2+ and La 3+ The co-doped CsPbCl3 nanocrystals exhibit a relatively weak reinforcing effect;

[0085] In Example 1, Mn 2+ and La 3+ Compared to Mn in Comparative Example 2, the co-doped CsPbCl3 nanocrystals... 2+ And Al 3+ Co-doping of Mn in Comparative Example 3 2+ and Ce 3+Co-doped CsPbCl3 nanocrystals exhibit a superior photoluminescence enhancement effect.

[0086] The above description of the embodiments is provided to enable those skilled in the art to understand and use the invention. It will be apparent to those skilled in the art that various modifications can be made to these embodiments, and the general principles described herein can be applied to other embodiments without inventive effort. Therefore, the present invention is not limited to the above embodiments, and any improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the invention should be within the protection scope of the present invention.

Claims

1. An orange-red light-emitting nanocrystal based on fluid channel reaction, characterized in that, The nanocrystals are nanocrystals co-doped with divalent manganese ions and trivalent lanthanum ions, synthesized by mixing and reacting a cesium oleate precursor solution and a lead-manganese-lanthanum source precursor solution through a fluid pipeline system. The nanocrystals are CsPbCl3, and the molar ratio of the lead source, manganese source and lanthanum source is 1:1:(0.1-1). The fluid piping system includes a preparation zone piping, a T-junction, and a reaction zone piping. The cesium oleate precursor solution and the lead-manganese-lanthanum source precursor solution flow into the preparation zone piping, are mixed through the T-junction, and are synthesized into nanocrystals through the reaction zone piping, respectively.

2. The orange-red light-emitting nanocrystal based on fluid channel reaction according to claim 1, characterized in that, The inner diameter of the pipeline in the preparation area is 700-900 μm, the outer diameter is 1400-1800 μm, and the length is 500-2000 mm. The inner diameter of the reaction zone pipe is 700-900 μm, the outer diameter is 1400-1800 μm, and the length is 200-300 mm.

3. A method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction as described in claim 1 or 2, characterized in that, The method includes the following steps: S1. Mix cesium source, oleic acid and octadecene, and heat under an inert gas atmosphere to obtain cesium oleate precursor solution; S2. Mix lead source, manganese source, lanthanum source, tri-n-octylphosphine and octadecene, heat under an inert gas atmosphere, add oleic acid and oleylamine, and continue heating under an inert gas atmosphere to obtain lead source-manganese source-lanthanum source precursor solution. S3. The cesium oleate precursor solution and the lead-manganese-lanthanum source precursor solution are mixed and reacted through a fluid pipeline system to obtain orange-red light-emitting nanocrystals based on fluid pipeline reaction.

4. The method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction according to claim 3, characterized in that, The cesium source in step S1 includes cesium carbonate or cesium acetate.

5. The method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction according to claim 3, characterized in that, In step S1, the molar / volume ratio of cesium source, oleic acid and octadecene is (1-5 mol):(1-5 L):(20-60 L).

6. The method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction according to claim 3, characterized in that, In step S2, lead chloride is used as the lead source, manganese chloride is used as the manganese source, and lanthanum chloride is used as the lanthanum source.

7. The method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction according to claim 3, characterized in that, In step S2, the molar / volume ratio of lead source, manganese source, tri-n-octylphosphine, octadecene, oleic acid and oleylamine is (0.1-0.4 mol):(0.1-0.4 mol):(1-4 L):(5-20 L):(1-2 L):(1-2 L).

8. The method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction according to claim 3, characterized in that, The heating temperature in step S1 is 100-140 ℃, and the time is 20-40 min.

9. The method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction according to claim 3, characterized in that, In step S2, the heating temperature after the first mixing and the heating temperature after the second addition are both 100-140 ℃. The heating time after the first mixing is 30-60 min, and the heating time after the second addition is 5-10 min.

10. The method for preparing orange-red light-emitting nanocrystals based on fluid channel reaction according to claim 3, characterized in that, The reaction temperature in step S3 is 170-210 ℃.

Citation Information

Patent Citations

  • Method for synergistically enhancing ultraviolet radiation stability and optical performance of Mn:CsPbCl3 nanocrystals

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