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Preparation method of energetic fullerene thin film in petal-shaped microstructure

A microscopic morphology, fullerene technology, applied in nanotechnology, organic chemistry, etc., can solve the problems of weakening the photoelectric properties of fullerene, high fullerene content, small specific surface area, etc., and achieve a simple, fast, high-rich preparation method The effect of the content of strene and large specific surface area

Inactive Publication Date: 2014-01-08
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Obtaining a large specific surface area and complex microscopic surface structure is particularly important for improving the performance of functional materials. It should be pointed out that in order to preserve the symmetrical structure of fullerene and its photoelectric properties to the greatest extent, generally pure fullerene or rich The self-assembled structure morphology is prepared by using derivatives with high content of slerene, but the obtained morphology is relatively simple, with small specific surface area, such as spherical, linear, rod-shaped and other shapes with smooth surface.
A recently reported fullerene derivative containing a long alkyl chain can self-assemble into a complex flower-like structure (Nakanishi T., et al, Small, 2007, 3, 2019–2023), but the disadvantage is that in this molecule The introduction of large substituents makes the content of fullerene itself in the obtained complex structure material less than 50%, which seriously weakens the photoelectric properties of fullerene itself
[0004] Therefore, it is still challenging for fullerene-based functional materials to ensure high fullerene content and controllable preparation of complex self-assembled structural film materials.

Method used

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  • Preparation method of energetic fullerene thin film in petal-shaped microstructure
  • Preparation method of energetic fullerene thin film in petal-shaped microstructure
  • Preparation method of energetic fullerene thin film in petal-shaped microstructure

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Experimental program
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Effect test

Embodiment 1

[0036] In a 100 ml single-necked volumetric flask, add 0.0582 g of C 60 , 0.0110 grams of p-nitrobenzaldehyde, 0.0381 grams of sarcosine and 30 milliliters of toluene, refluxed at 115 ° C for 5 hours under the protection of nitrogen, the color of the solution changed from purple to brown. Concentrate with a vacuum rotary evaporator and then purify by silica gel column chromatography, the eluent is toluene and n-hexane (volume ratio 20:1). The resulting product was recrystallized from chloroform and isopropanol (volume ratio 25:3) to obtain nitrophenyl-substituted fullerene derivatives. Characterized by MALDI-TOF-MS, m / z calcd 897.8; found 896.8 (100%).

Embodiment 2

[0038] Self-assembly of fullerene derivatives on solid substrates and preparation of energetic fullerene films with petal-like microscopic morphology.

[0039] Cut the solid substrate into square pieces of about 0.25 cm2 with a glass knife (for monocrystalline silicon) or scissors (for nylon, ginkgo leaves and camphor leaves), rinse the surface with acetone, and dry naturally; take out 20 Microliter 1 mg / ml fullerene derivative in chloroform-ethanol (volume ratio 10:1) solution, or 20 microliter 1 mg / ml fullerene derivative in chloroform-n-hexane (volume ratio 10:1) solution , were directly dropped on a clean solid substrate, and evaporated to dryness naturally; the substrate with the fullerene self-assembled structure was sprayed with gold for 20 seconds, and the fullerene film was observed by Hitachi TM-1000 scanning electron microscope petal-like microstructure.

Embodiment 3

[0041] Preparation of energetic fullerene films with petal-like microscopic morphology on single crystal silicon substrates.

[0042] Cut the solid substrate monocrystalline silicon into square pieces of about 0.25 cm2 with a glass knife, rinse the surface with acetone, and let it dry naturally; use a pipette gun to take out 20 μl of 1 mg / ml fullerene derivative in chloroform-ethanol ( 10:1 by volume) solution, or 20 microliters of 1 mg / ml fullerene derivative in chloroform-n-hexane (10:1 by volume) solution, were directly dropped on the clean solid substrate single crystal silicon, and naturally Evaporate until dry; spray gold on the substrate with fullerene self-assembled structure for 20 seconds, and observe with a Hitachi TM-1000 scanning electron microscope, you can see the petal-shaped microscopic morphology of the fullerene film material.

[0043] The scanning electron micrograph of the petal-shaped microscopic morphology of the fullerene film obtained from the chlorofo...

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Abstract

The invention relates to a preparation method of an energetic fullerene thin film in a petal-shaped microstructure. The preparation method comprises the steps of (1) in nitrogen protection, implementing reflux reaction to fullerene C60, p-nitrobenzaldehyde and sarcosine in an organic solvent, concentrating, separating and purifying, and recrystallizing to obtain a N-methyl-2-(4-nitrophenyl) [60] fullerene pyrrolidine derivative; (2) dissolving the N-methyl-2-(4-nitrophenyl) [60] fullerene pyrrolidine derivative in an organic solvent, dropping on a substrate, naturally drying and self-assembling to obtain the energetic fullerene thin film in the petal-shaped microstructure. The fullerene derivative obtained from the preparation method is high in fullerene content, rapid and simple in preparation method, and wide in the adopted substrate and contains energetic group nitro; the fullerene thin film material in the petal-shaped microstructure can be prepared in a large area, and has potential application prospect in catalytic materials, photoelectrical materials, energy storage materials and other fields.

Description

technical field [0001] The invention belongs to the field of preparation of nano film materials, in particular to a preparation method of an energy-containing fullerene film with petal-like microscopic appearance. Background technique [0002] The unique spherical π-electron structure and photoelectric properties make fullerenes (C 60 ) has attracted much attention in the field of materials science (Dubacheva G.V., et al, Coord. Chem. Rev., 2012, 256, 2628–2639). Recent studies have found that by controlling the key structural unit C in photoelectric conversion and catalytic functional materials 60 The self-assembled structure morphology is one of the important ways to effectively improve the performance of functional materials (Guld D.M., et al, Chem. Soc. Rev., 2009, 38, 1587–1597). At present, many studies have reported that by modifying C 60 The surface achieves control of its self-assembled structure morphology, such as in different C 60 Among derivatives, spherical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/70B82Y40/00
CPCC07D209/96B82Y40/00
Inventor 张煊李旭东
Owner DONGHUA UNIV
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