Preparation method of hybrid material compounded from fullerene micro-nano material and conjugated polymer

A conjugated polymer and hybrid material technology, which is applied in the field of hybrid material preparation of fullerene-based micro-nano materials and conjugated polymers, can solve difficult large-scale preparation, complex preparation technology, and poor purity control problem, to achieve the effect of short production cycle, simple overall process and reliable principle

Active Publication Date: 2013-11-27
QINGDAO UNIV OF SCI & TECH
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Problems solved by technology

[0003] However, the above-mentioned methods have problems such as small aspect ratio of the obtained sample, poor control of purity, complicated preparation technology, etc.
In recent years, Japanese Laid-Open Patents 2005-254393A and 2006-124266A have disclosed 60 Preparation of fullerene C with single crystal structure by liquid-liquid interfacial precipitation from saturated organic solution and isopropanol 60 Nanowhiskers and nanotubes, the nanofibers synthesized by this method have a single crystal structure, high aspect ratio and high purity (99.9%), however, the problem of this method is the preparation of fullerene C 60 and C 70 The nanotubes have a long growth period (more than one week), and poor reproducibility, so it is difficult to prepare on a large scale; in view of these problems, Chinese patent CN100581998C discloses a simple, easy, repeatable, suitable for mass production, has a single crystal structure, high Template-free preparation method of solid or hollow fullerene-based micro-nanofibers with aspect ratio and high purity
[0005] Conductive polymers have been a hot research topic in the field of materials in recent years, but the conductivity of such conductive polymers is relatively low in the intrinsic state, and they must be doped to have good conductivity; fullerenes are good electron acceptors. body, and the conjugated polymer contains atoms with lone pairs of electrons, which are electron donors, so the conjugated polymer can be doped with fullerene molecules to increase its conductivity; about the preparation of the original fullerene powder and the conjugated Conjugated polymer hybrid materials have been reported endlessly, such as Wang et al. (Wang Q, Wang S, Li J, et al. J. Polym. ) with C 60 Powder and aniline were used as raw materials to prepare C 60 / PANI COMPOSITE, in C 60 And under a certain ratio of polyaniline, the electrical conductivity of the composite material is good; I.Sapurina et al. -2326) by adding C 60 Doping into polyaniline increases the thermal stability and conductivity of polyaniline, but these methods only use the properties of fullerene electron acceptors, and use it to dope conjugated polymers to increase their conductivity. This kind of doping is relatively expensive. If the fullerene-based micro-nano material prepared by the original fullerene powder can be hybridized with the conjugated polymer, the morphology of the fullerene-based micro-nano fiber / chip can be made Great changes have taken place, and at the same time, the conductivity of conjugated polymers has been improved by doping. Such recombination can obtain nano-hybrid materials with brand-new opto-electromagnetic and mechanical properties.

Method used

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Examples

Experimental program
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Embodiment 1

[0015] The preparation process steps of the present embodiment include:

[0016] (1) Weigh 14mg C 60 Powder, after being ground, dissolved in 5ml of toluene, ultrasonicated for 10min in an ice bath; after filtering the above solution, 5ml of isopropanol was added to it at a volume ratio of 1:1, and placed in a constant temperature incubator for 24 hours at a constant temperature of 4°C to prepare Fullerene micro-nanofibers (FM / NFs) with a length of 10-20 μm;

[0017] (2) Measure 1.8ml of aniline (An) and add it to 100ml of HCl with a concentration of 1mol / L, mix and stir; then add 1.14g of ammonium persulfate (APS) to the above solution, stir for 1min, and put it in the refrigerator to control the temperature Refrigerate at -12°C for 12 hours, add 45ml of ammonia water with a concentration of 1.74mol / L and soak for 5 minutes after suction filtration, dry to obtain PANI-EB powder, grind it for use;

[0018](3) Dissolve PANI-EB powder in N-methyl-2-pyrrolidone (N-methyl-2-pyrr...

Embodiment 2

[0021] This example is the same as Example 1. The liquid-liquid interface method is used to prepare fullerene micro-nano materials. The difference is that the good solvents are pyridine, pyridinone, benzene, carbon disulfide, aniline and ethanol. The prepared materials are Different body shapes, including flakes and pellets.

Embodiment 3

[0023] The difference between this embodiment and the steps of Example 1 is that in the preparation of fullerene micro-nano materials, evaporation C 60 - Saturated solution of toluene, C 60 - Benzene saturated solution and C 60 -The method of saturated solution of dichlorobenzene, i.e. evaporation method, is prepared.

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Abstract

The invention belongs to the technical field of material preparation, and relates to a preparation method of a hybrid material compounded from a fullerene micro-nano material and a conjugated polymer. The preparation method comprises the following steps: placing a fullerene substance into a agate mortar for grinding; dissolving the fullerene substance by adopting a good solvent, and then removing into a transparent glass bottle; carrying out ultrasonic dispersion by using ultrasonic waves in an ice-water bath, then filtering at room temperature to obtain a fullerene saturated solution, and then culturing by adding isopropanol to obtain suspending liquid which contains the fullerene micro-nano material; dissolving the conjugated polymer into the good solvent, and filtering to obtain a conjugated polymer solution; adding the conjugated polymer solution to the suspending liquid which has the volume ratio of 1-10 times and contains the fullerene micro-nano material; and carrying out oscillating mixing processing by using the ultrasonic waves, and culturing to obtain the hybrid material compounded from the fullerene micro-nano material and the conjugated polymer. The preparation method disclosed by the invention has the advantages of simple integral process, reliability in principle and short production period; the prepared material has the advantages of good property, wide application range, high reliability and environment friendliness.

Description

Technical field: [0001] The invention belongs to the technical field of material preparation, and relates to a composite modification technology of fullerene-based micro-nano materials, in particular to a method for preparing a hybrid material in which fullerene-based micro-nano materials are compounded with conjugated polymers. Background technique: [0002] Low-dimensional micro-nano carbonaceous materials are ideal systems for studying physical properties such as electron transport behavior, optical properties, and mechanical properties. They will play an important role in the research fields of integrated circuits and functional components such as micro-nano electronics and optoelectronic devices. Realizing the expansion of its application and diversification of functions, and the modification of low-dimensional nano-carbon structure materials have become a hot issue in the current scientific research of micro-nano materials. In 1985, Kroto et al. discovered the fulleren...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L79/02C08L79/04C08L65/00C08K9/04C08K9/02C08K3/04
Inventor 朴光哲高鑫王冰哲
Owner QINGDAO UNIV OF SCI & TECH
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