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Method for increasing manganese doping concentration and light emission efficiency of manganese-doped CsPbCl3 nanocrystal

A technology of luminous efficiency and manganese doping, applied in nano optics, nanotechnology, luminescent materials, etc., to achieve the effect of improving luminous efficiency

Active Publication Date: 2019-09-10
JILIN NORMAL UNIV
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Problems solved by technology

[0003] In existing studies, at a relatively low synthesis temperature of 190 °C, CsPbCl 3 Mn in nanocrystals 2+ The doping concentration is generally at the level of 1% to 7%, and to obtain the highest point of 7%, the molar ratio of Mn to Pb needs to be 5:1, as shown in the literature (Chem.Mater.2017, 29, 8003-8011 ), if you want in CsPbCl 3 Achieve up to 15% Mn in nanocrystals 2+ The doping concentration needs to increase the synthesis temperature to 210 or 230 °C, as documented (Chem. Mater. Increased CsPbCl at a lower synthesis temperature of 190°C 3 Mn in nanocrystals 2+ CsPbCl can be achieved under the condition of doping concentration or lower synthesis temperature 3 Up to 15% Mn in nanocrystals 2+ Doping concentration has become an urgent problem for researchers to solve
[0004] In addition, in existing studies, such as those reported by Samanta et al. (Nanoscale2017, 9, 16722-16727), Pradhan et al. (J. Phys. Chem. Lett. 2019, 10, 1530-1536) and our previous experimental results show that (Chem.Mater.2017,29,8003-8011), manganese doped CsPbCl 3 The luminous efficiency of nanocrystals in orange light (600nm) and red light (620nm) is about 60% and 10%

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  • Method for increasing manganese doping concentration and light emission efficiency of manganese-doped CsPbCl3 nanocrystal
  • Method for increasing manganese doping concentration and light emission efficiency of manganese-doped CsPbCl3 nanocrystal
  • Method for increasing manganese doping concentration and light emission efficiency of manganese-doped CsPbCl3 nanocrystal

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[0028] The present invention provides a kind of by introducing NiCl 2 Improve Mn-doped CsPbCl 3 A preparation method for doping and luminous efficiency of nanocrystals, the method comprising:

[0029] Step 1: Mix cesium carbonate, oleic acid and an oil phase solvent, and under the protection of an inert gas, stir and heat until the solution is clarified to obtain a cesium precursor solution, which is cooled to 100°C for use. The molar mass of the cesium carbonate is 0.68mmol, and the oil phase solvent is preferably one or more of octadecylamine, octadecene, oleylamine, more preferably octadecene; oleic acid and oil phase solvent The volume ratio is preferably 1:(6~10), more preferably 1:8; the inert gas is preferably nitrogen, helium, neon or argon, more preferably argon; the heating temperature is 130 ~170°C, more preferably 150°C for 5 minutes.

[0030] Step 2: Mix octadecene, oleic acid, oleylamine, trioctylphosphine, lead chloride, manganese chloride and nickel chloride...

Embodiment 1

[0035] Step 1: join 0.68mmol cesium carbonate, 1.25mL oleic acid, 10mL octadecene in the three-necked bottle of 50mL at room temperature, vacuumize, feed inert gas, to remove gas, under the protection of argon, will Stir and heat the mixed solution to 150°C, and keep this temperature until the solution is clear and transparent to obtain a cesium precursor solution, and cool it to 100°C for use; the number of vacuum pumping can be multiple times, specifically 2, 3, or 4 times Wait;

[0036] Step 2: Add 5mL octadecene, 1.5mL oleic acid, 1.5mL oleylamine, 1mL trioctylphosphine, 0.2mmol lead chloride, 0.2mmol manganese chloride and 0.2mmol nickel chloride into a 50mL three-necked bottle, Vacuumize and introduce inert gas to remove gas. Under the protection of argon, stir and heat the mixed solution to 190°C, and keep this temperature for 10min to fully dissolve nickel chloride; the number of times of vacuuming can be multiple, Specifically, it can be 2 times, 3 times, 4 times, et...

Embodiment 2

[0040] Step one: at room temperature, 0.68mmol cesium carbonate, 1.25mL oleic acid, 8mL octadecylamine are added in the three-necked bottle of 50mL, vacuumize, feed inert gas, to remove gas, under the protection of nitrogen, will The mixed solution is stirred and heated to 130°C, and kept at this temperature until the solution is clear and transparent to obtain a cesium precursor solution, which is cooled to 100°C for use; the number of vacuum pumping can be multiple times, specifically 2, 3, or 4 times Wait;

[0041] Step 2: Add 5mL octadecene, 1.5mL oleic acid, 1.5mL oleylamine, 1mL trioctylphosphine, 0.2mmol lead chloride, 0.2mmol manganese chloride and 0.2mmol nickel chloride into a 50mL three-necked bottle, Vacuumize and introduce inert gas to remove gas. Under the protection of nitrogen, stir and heat the mixed solution to 190°C, and keep this temperature for 10min to fully dissolve nickel chloride; the number of times of vacuuming can be multiple, the specific It can b...

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Abstract

The invention relates to the technical field of CsPbCl3 nanocrystal material preparation and in particular to a method for increasing the manganese doping concentration and the light emission efficiency of a manganese-doped CsPbCl3 nanocrystal. The method comprises the following steps: preparing a caesium precursor solution; mixing octadecene, oleic acid, oleylamine, tri-n-octylphosphine, lead chloride, lead chloride, manganese chloride and nickel chloride; and forming a Ni-Mn double-doped CsPbCl3 nanocrystal, so as to obtain a Ni-Mn double-doped CsPbCl3 nanocrystal solution. By adopting the method, by adding NiCl2, the crystallinity and the surface defect state of a Mn-doped CsPbCl3 nanocrystal can be improved, the doping concentration of Mn in the manganese-doped CsPbCl3 nanocrystal canbe increased, and the light emission efficiency of the manganese-doped CsPbCl3 nanocrystal can be improved.

Description

technical field [0001] The present invention belongs to doped CsPbCl 3 The technical field of nanocrystalline material preparation, specifically related to a method of improving manganese-doped CsPbCl 3 Methods of manganese doping concentration and luminous efficiency of nanocrystals. Background technique [0002] mn 2+ doped CsPbCl 3 Nanocrystals with a broad orange-red emission were first reported in 2016 to combine Mn 2+ Doping into perovskite makes it a potential application in next-generation white LEDs. As we all know, Mn 2+ :CsPbCl 3 The yellow-orange emission in nanocrystals comes from CsPbCl-based 3 Mn 2+ Mn dopant energy transfer 2+ ion 4 T 1 → 6 A 1 d~d transition. mn 2+ :CsPbCl 3 The yellow-orange glow of nanocrystals comes from isolated Mn 2+ The ion has an orange emission (-590-600 nm), showing a high photoluminescence yield up to about 60%. And some red Mn 2+ :CsPbCl 3 The luminescence of nanocrystals comes from Mn 2+ ~Mn 2+ For red emiss...

Claims

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Application Information

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IPC IPC(8): C09K11/66B82Y20/00B82Y30/00B82Y40/00
CPCC09K11/665B82Y20/00B82Y30/00B82Y40/00
Inventor 袁曦赵家龙邢柯李海波
Owner JILIN NORMAL UNIV
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