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Preparation method of fullerene derivative film with micron flower shape

A technology of fullerene derivatives and methylene fullerene, which is applied in the direction of hydrocarbon production from halogen-containing organic compounds, nanotechnology, organic chemistry, etc., can solve the problems of reducing the electron transmission efficiency of C60, and achieve high utilization rate , The preparation process is simple, the effect of large specific surface area

Inactive Publication Date: 2019-04-09
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the introduction of N atoms containing lone pairs of electrons in these compounds, there is electronic interaction with the fullerene carbon cage, which reduces the C 60 The electron transfer efficiency of

Method used

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  • Preparation method of fullerene derivative film with micron flower shape
  • Preparation method of fullerene derivative film with micron flower shape
  • Preparation method of fullerene derivative film with micron flower shape

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 144mg C 60 Place in a 500mL custom-made three-port electrolytic cell, and add 100mL of benzonitrile solution containing 0.1M tetrabutylammonium perchlorate (TBAP). The glassy carbon electrode is used as the working electrode, the platinum mesh electrode is used as the counter electrode, and the saturated calomel electrode is used as the reference electrode, respectively inserted into the electrolytic cell. Magnetic stirring, under the protection of nitrogen, controlled potential electrolysis at -1.1V voltage to electrolysis, the solution gradually changed from lavender to dark red. to C 60 is fully electrolyzed C 60 2- , to stop electrolysis. Quickly add 10-50 times of PhCHBr to the reaction solution 2 , the solution changed from dark red to dark green, and then gradually turned to brownish yellow. The reaction was stirred vigorously for 50 min, and the reaction was stopped. The reaction solution was transferred to a round bottom flask, and the solvent was ...

Embodiment 2

[0035] Accurately weigh 20mg of 1,2-(phenyl)methylenefullerene C 60 , placed in a 25mL ground-neck Erlenmeyer flask, add 10mL of m-xylene, ultrasonically dissolve for 5min, and make 2mg / mL of 1,2-(phenyl)methylenefullerene C 60 - m-xylene solution, set aside. Cut glass slides into 1cm×1cm squares with a glass knife, ultrasonically clean them three times with acetone, deionized water, and ethanol, and finally dry them with nitrogen. Use a pipette gun to accurately pipette 20 μL of the above 2 mg / mL 1,2-(phenyl)methylenefullerene C 60 -Meta-xylene solution, drop-coated on the surface of the glass sheet, and let it dry naturally. For SEM testing such as figure 2 .

[0036] The prepared 1,2-(phenyl)methylenefullerene C 60 The glass sheet film was placed in a muffle furnace, heated to 330°C, kept at the temperature for 10 minutes, and then lowered to room temperature. Scanning electron microscope tests such as Figure 4 .

Embodiment 3

[0038] Accurately pipette 10 μL of the 2 mg / mL 1,2-(phenyl)methylenefullerene C of Example 2 with a pipette gun 60 -Meta-xylene solution, drop-coated on the copper grid. Allow to dry for TEM testing such as image 3 .

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Abstract

The present invention relates to a kind of preparation method of the fullerene derivative thin film of micron flower shape shape, 1,2-(phenyl) methylene fullerene C 60 dissolved in a solvent, and the resulting 1,2‑(phenyl)methylenefullerene C 60 ‑Meta-xylene solution, drop-coated on the substrate, and let it dry naturally at room temperature to obtain a fullerene derivative film with micron flower-like morphology. The present invention introduces a relatively small (phenyl) methylene group on the fullerene molecule, and more than 90% of the fullerene molecule is retained, which not only increases the solubility of the fullerene molecule, but also relatively maintains Excellent properties of fullerenes. The micron flower-like fullerene film of the invention has good dispersibility, simple and fast preparation process, and can be prepared in a large area at room temperature. It is expected to be used in light-emitting devices, solar cells and other fields.

Description

technical field [0001] The invention relates to the field of preparation of nano film materials, in particular to a preparation method of a fullerene derivative film with a micron flower shape. Background technique [0002] Due to its unique three-dimensional structure and strong ability to accept electrons, fullerene C 60 It has received widespread attention since its discovery. Fullerenes have shown potential applications in solar cells, organic photoelectric transfer tubes, sensors, and biomedicine. Studies have shown that the microstructure and morphology of fullerenes have an important impact on their properties. For example, the photoelectric conversion efficiency of organic heterojunction solar cells largely depends on the microscopic morphology of the photoactive fullerene layer (Huang, Y. et al Chem. Rev., 2014, 114, 7006). Therefore, the C 60 The controllable assembly of micro-nanomaterials with specific structures has aroused widespread interest of scientific ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C1/28C07C13/16B82Y40/00
CPCB82Y40/00C07C1/28C07C13/16
Inventor 常伟伟
Owner SHANDONG UNIV OF TECH
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