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Preparation method of organic-inorganic hybrid halide micro-nano tubes

A technology of micro-nanotubes and halides, which is applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of zero-dimensional organic-inorganic hybrid halide controllable morphology micro-nanotubes that have not been reported, and achieve the goal of overcoming the morphology Uncontrollable size, very high confinement effect, high purity effect

Inactive Publication Date: 2020-02-21
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, thermal injection is used for (C 5 h 7 N 2 ) 2 ZnBr 4 The synthesis of this class of zero-dimensional organic-inorganic hybrid halide micro-nanotubes with controllable morphology has not been reported yet.

Method used

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  • Preparation method of organic-inorganic hybrid halide micro-nano tubes
  • Preparation method of organic-inorganic hybrid halide micro-nano tubes
  • Preparation method of organic-inorganic hybrid halide micro-nano tubes

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1 (C 5 h 7 N 2 ) 2 ZnBr 4 Preparation of micro-nanotubes

[0040] Put 0.1mmol of anhydrous zinc acetate, 0.2mmol of 4-aminopyridine, 10ml of octadecene, 2.0mL of oleic acid and 0.2mL of oleylamine into a three-necked bottle and accompanied by strong magnetic stirring, under the protection of nitrogen The temperature was gradually raised to 110°C and kept for 1 hour. The solution was a light yellow clear solution. Then the temperature was naturally lowered to 80°C and kept for 30 minutes. Added 0.1 mL of bromotrimethylsilane with a concentration of 98%, the solution quickly turned into a white suspension. show (C 5 h 7 N 2 ) 2 ZnBr 4 micronanotube formation. Take it out after 8 minutes and wash the sample twice with toluene. Such as figure 1 As shown, (C 5 h 7 N 2 ) 2 ZnBr 4 The X-ray diffraction pattern (XRD) of the micro-nanotubes fits very well with the theoretically calculated XRD. figure 2 Scanning electron micrographs with a scale bar ...

Embodiment 2

[0041] Embodiment 2 reduces temperature and is 60 ℃ (C 5 h 7 N 2 ) 2 ZnBr 4 Preparation of micro-nanotubes

[0042] Put 0.1mmol of anhydrous zinc acetate, 0.2mmol of 4-aminopyridine, 10ml of octadecene, 2.0mL of oleic acid and 0.2mL of oleylamine into a three-necked bottle and accompanied by strong magnetic stirring, under the protection of nitrogen The temperature was gradually raised to 110°C and kept for 1 hour. The solution was a light yellow clear solution. Then the temperature was naturally lowered to 60°C and kept for 30 minutes. Added 0.1 mL of bromotrimethylsilane with a concentration of 98%, the solution gradually turned into a white suspension. show (C 5 h 7 N 2 ) 2 ZnBr 4 micronanotube formation. Take it out after 8 minutes and wash the sample twice with toluene. Figure 5 The scanning electron micrographs with a scale bar of 50 μm are more uniform in size compared with those at 80°C. Figure 6~7 Scanning electron micrographs with scale bars of 10 μm an...

Embodiment 3

[0043] Embodiment 3 increases the amount of oleylamine to be 0.5mL (C 5 h 7 N 2 ) 2 ZnBr 4 Preparation of micro-nanotubes

[0044] Put 0.1mmol of anhydrous zinc acetate, 0.2mmol of 4-aminopyridine, 10ml of octadecene, 2mL of oleic acid and 0.5mL of oleylamine into a three-necked flask accompanied by strong magnetic stirring, and bring the temperature under the protection of nitrogen. Gradually rise to 110°C and keep it for 1h, the solution is a light yellow clear solution, then naturally cool down to 80°C, keep it for 30min, add 0.1mL trimethylbromosilane with a concentration of 98%, the solution quickly turns into a white suspension, showing (C 5 h 7 N 2 ) 2 ZnBr 4 micronanotube formation. Take it out after 8 minutes and wash the sample twice with toluene. Such as Figure 8-9 As shown, the product changes from micro-nanotubes to ellipsoidal nanotubes with an increase in the amount of oleylamine, and the average diameter of the ellipsoidal tubes is 500 μm.

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Abstract

The invention discloses a preparation method of organic-inorganic hybrid halide micro-nano tubes, and belongs to the technical field of preparation of semiconductor micro-nano tube materials. The preparation method comprises following steps: introducing 4-aminopyridine, anhydrous zinc acetate, octadecene, oleic acid and oleylamine into a three-necked bottle, magnetically stirring, heating to 110 DEG C under the protection of nitrogen gas, keeping the temperature for 1 hour, naturally cooling to 80-60 DEG C, keeping the temperature for 30 minutes, injecting trimethylbromosilane, and convertingan obtained solution into a white turbid solution, thereby obtaining the (C5H7N2)2ZnBr4 micro-nano tubes. By changing the volume ratio or the reaction temperature of oleic acid to oleylamine, the sizeand the morphology of the (C5H7N2)2ZnBr4 micro-nano tubes can be controlled. Synthesis of the micro-nano tubes in organic-inorganic hybrid halides is realized for the first time, the vacancy of the halide synthesis technology is filled, and conditions are provided for research in the field of luminescent materials.

Description

technical field [0001] The invention belongs to the technical field of semiconductor micro-nano tube material preparation, and in particular relates to a method for preparing high-purity micro-nano tube and controlling its shape. Background technique [0002] The U.S. Energy Information Administration reports that 21 percent of all energy consumed in the U.S. in 2017 was used for lighting. Replacing incandescent bulbs with light-emitting diodes (LEDs) is expected to reduce power consumption by 40% by 2030. To achieve this goal, scientists are working on developing entirely new material technologies that can generate finely tuned white light (WL). The development of white light (WLED) is a key step in the implementation of solid-state lighting (SSL) technology, which promises to solve the inefficiency of traditional incandescent and fluorescent light sources. In order to generate white light (WL), the commonly used technology is to coat LEDs with phosphor or mix LEDs of mul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C09K11/61
CPCC09K11/06C09K11/615
Inventor 肖冠军赵电龙马志伟刘锦阳邹勃
Owner JILIN UNIV
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