JP2004352608A - Method for dispersing carbon nano-structure - Google Patents
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Abstract
Description
本発明は、炭素ナノ構造体（carbon nano-strucutre）の表面をフッ素化する方式で溶媒中での炭素ナノ構造体の分散性を改善する方法に関する。 The present invention relates to a method for improving the dispersibility of a carbon nano-structure in a solvent by fluorinating the surface of the carbon nano-structure.
炭素ナノ繊維、フラーレン、炭素ナノチューブおよび炭素ナノホーンのような炭素ナノ構造体は、これらの優れた物理的、化学的および電気的特性によって、電磁波遮蔽、電子装置または無機−有機複合体などの様々な分野に用いられている。 Carbon nanostructures, such as carbon nanofibers, fullerenes, carbon nanotubes and carbon nanohorns, can be used in various fields such as electromagnetic wave shielding, electronic devices or inorganic-organic composites due to their excellent physical, chemical and electrical properties. Used in the field.
しかし、このような炭素ナノ構造体は基質中に混入されると凝集し、そのユニークな特性が劣化する傾向にある。したがって、基質中で凝集しない分散性のよい炭素ナノ構造体を開発しようとする多くの試みがあった。 However, such carbon nanostructures tend to aggregate when mixed into a substrate, deteriorating their unique properties. Therefore, there have been many attempts to develop carbon nanostructures with good dispersibility that do not aggregate in the substrate.
たとえば、界面活性剤を用いて炭素ナノチューブを溶媒中に分散する方法が開示されているが（特許文献１参照）、この方法では完全に分散された炭素ナノチューブ分散液が得られない。 For example, a method of dispersing carbon nanotubes in a solvent using a surfactant has been disclosed (see Patent Document 1), but this method does not provide a completely dispersed carbon nanotube dispersion.
そこで、本発明者らは、炭素ナノ構造体を表面処理することによって、炭素ナノ構造体の分散性を改善させるための方法を開発することによって本発明を完成した。
したがって、本発明の目的は、炭素ナノ構造体を溶媒中に個別的に分離させるのに効果的な方法を提供することである。 Therefore, an object of the present invention is to provide an effective method for individually separating carbon nanostructures in a solvent.
本発明の一実施態様によって、本発明では、炭素ナノ構造体の表面を含フッ素ガスでフッ素化処理した後、フッ素化処理された炭素ナノ構造体を溶媒中に分散させることを含む、炭素ナノ構造体の分散方法が提供される。 According to one embodiment of the present invention, the present invention provides a method for producing a carbon nanostructure, comprising: fluorinating the surface of a carbon nanostructure with a fluorine-containing gas, and then dispersing the fluorinated carbon nanostructure in a solvent. A method for dispersing a structure is provided.
本発明によれば、分散前にフッ素化処理された炭素ナノ構造体は均一な粒子サイズで溶媒中に分散できる。 According to the present invention, a carbon nanostructure that has been fluorinated before dispersion can be dispersed in a solvent with a uniform particle size.
以下、本発明をさらに詳細に説明する。
本発明に係る方法は、炭素ナノ構造体を分散前に予めフッ素化処理することを特徴とする。
Hereinafter, the present invention will be described in more detail.
The method according to the present invention is characterized in that the carbon nanostructure is preliminarily fluorinated before being dispersed.
図１に概略的に示すように、本発明の一実施態様によれば、炭素ナノ構造体を必要に応じて精製し、フッ素化処理（Ｓ１０）した後、フッ素化処理された炭素ナノ構造体を溶媒に分散させる（Ｓ２０）。任意に、フッ素化処理された炭素ナノ構造体分散液を超音波処理し（Ｓ３０）、酸やアルカリ溶液を用いて分散液のｐＨを目的とする範囲に調節する（Ｓ４０）。その後、本発明の分散方法によって得られた炭素ナノ構造体分散液の分散度を分析する（Ｓ５０）。 As schematically shown in FIG. 1, according to one embodiment of the present invention, the carbon nanostructure is purified if necessary, fluorinated (S10), and then fluorinated. Is dispersed in a solvent (S20). Optionally, the fluorinated carbon nanostructure dispersion is subjected to ultrasonic treatment (S30), and the pH of the dispersion is adjusted to a target range using an acid or alkali solution (S40). Then, the degree of dispersion of the carbon nanostructure dispersion obtained by the dispersion method of the present invention is analyzed (S50).
具体的に、本発明の方法において、分散される炭素ナノ構造体としては、公知の合成法、たとえば、化学蒸着法（ＣＶＤ）、アーク（arc）法、レーザ・アブレーション（laser ablation）などによって合成されたどのような種類の炭素ナノ構造体も用いられる。 Specifically, in the method of the present invention, the carbon nanostructure to be dispersed may be synthesized by a known synthesis method, for example, a chemical vapor deposition method (CVD), an arc method, an laser ablation method, or the like. Any type of carbon nanostructure that has been used can be used.
このような炭素ナノ構造体は、場合に応じて公知の方法、たとえば、４００〜８００℃の空気のような酸化ガス雰囲気中で熱処理するか、塩酸、硝酸、フッ酸または硫酸のような無機強酸で処理することによって、非晶質炭素または触媒金属を除去して精製してもよい。 Such a carbon nanostructure may be heat-treated in a known manner, for example, in an oxidizing gas atmosphere such as air at 400 to 800 ° C., or may be an inorganic strong acid such as hydrochloric acid, nitric acid, hydrofluoric acid or sulfuric acid. , The amorphous carbon or the catalytic metal may be removed for purification.
本発明によれば、精製されたか、または精製されていない炭素ナノ構造体を−２０〜５００℃でフッ素ガスで処理する。前記フッ素ガスは、炭素に対するフッ素の原子比が０．００１〜５０：１００、好ましくは０．００１〜３０：１００、さらに好ましくは０．００１〜５：１００の範囲の量で使用する。このようなフッ素化処理によって、フッ素基が炭素ナノ構造体の表面の一部を覆うことによって、溶媒中で炭素ナノ構造体粒子の粒子間の相互作用を減少させて炭素ナノ構造体の凝集を抑制する。フッ素化処理された炭素ナノ構造体は個別粒子（単一壁炭素ナノチューブの場合、粒子サイズが１〜３ｎｍである）として溶媒中に分散され、炭素ナノ構造体自体のユニークな特徴が発揮できる。 According to the present invention, the purified or unpurified carbon nanostructure is treated with fluorine gas at -20 to 500C. The fluorine gas is used at an atomic ratio of fluorine to carbon of 0.001 to 50: 100, preferably 0.001 to 30: 100, and more preferably 0.001 to 5: 100. By such a fluorination treatment, the fluorine group covers a part of the surface of the carbon nanostructure, thereby reducing the interaction between the carbon nanostructure particles in the solvent and reducing the aggregation of the carbon nanostructure. Suppress. The fluorinated carbon nanostructure is dispersed in a solvent as individual particles (in the case of a single-walled carbon nanotube, the particle size is 1 to 3 nm), and the unique characteristics of the carbon nanostructure itself can be exhibited.
本発明において、マトリックスとして使用され得る溶媒の例としては、蒸留水、イソプロパノール、ジメチルホルムアミド、クロロホルム、ジクロロエタン、メチルピロリドン、テトラヒドロフラン、デカンまたはこれらの混合物がある。 In the present invention, examples of solvents that can be used as a matrix include distilled water, isopropanol, dimethylformamide, chloroform, dichloroethane, methylpyrrolidone, tetrahydrofuran, decane or a mixture thereof.
前記溶媒は、分散剤として任意に界面活性剤、水溶性高分子またはこれらの混合物を、溶媒に対して０．００１〜５．０重量％の量で含んでもよい。界面活性剤および水溶性高分子は、好ましくは１：０．８の重量比で混合してもよい。 The solvent may optionally contain a surfactant, a water-soluble polymer or a mixture thereof as a dispersant in an amount of 0.001 to 5.0% by weight based on the solvent. The surfactant and the water-soluble polymer may be mixed preferably in a weight ratio of 1: 0.8.
前記界面活性剤の例としては、ドデシル硫酸ナトリウム、ドデシルベンゼン硫酸ナトリウム、ブチルベンゼン硫酸ナトリウム、臭化ドデシルトリメチルアンモニウム、トリトン（Triton）Ｘ−１００、塩化ベンズアルコニウムまたはこれらの混合物がある。 Examples of the surfactant include sodium dodecyl sulfate, sodium dodecyl benzene sulfate, sodium butyl benzene sulfate, dodecyl trimethyl ammonium bromide, Triton X-100, benzalkonium chloride or a mixture thereof.
前記水溶性高分子の例としては、アカシア、シクロデキストリン、ポリビニルピロリドン、カルボキシルメチルセルロースまたはこれらの混合物がある。 Examples of the water-soluble polymer include acacia, cyclodextrin, polyvinylpyrrolidone, carboxymethylcellulose or a mixture thereof.
本発明の方法において、炭素ナノ構造体分散液を場合に応じて１００〜７５０Ｗの超音波で１０分〜２時間処理して炭素ナノ構造体の分散を促進できる。 In the method of the present invention, the dispersion of the carbon nanostructure can be promoted by treating the carbon nanostructure dispersion liquid with ultrasonic waves of 100 to 750 W for 10 minutes to 2 hours as appropriate.
さらに、場合に応じて、炭素ナノ構造体分散液に酸またはアルカリ溶液を添加して分散液のｐＨを８〜１４の範囲に調節することによって分散効果を高めることができる。 Further, if necessary, an acid or alkali solution is added to the carbon nanostructure dispersion to adjust the pH of the dispersion to a range of 8 to 14, so that the dispersion effect can be enhanced.
（実施例）
以下、本発明を下記実施例によってさらに詳細に説明する。ただし、これらは本発明を例示するためのものであり、本発明の範囲を制限しない。
(Example)
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, these are only for illustrating the present invention, and do not limit the scope of the present invention.
［実施例１］
通常のＣＶＤ方法で合成した単一壁炭素ナノチューブを、管状反応器を用いて４００℃の温度で空気で酸化処理することによって精製した。精製された炭素ナノチューブをさらに０．１ｂａｒのフッ素ガス（Ｆ2）の雰囲気下、４０℃で３０分間フッ素化処理した。フッ素化処理された炭素ナノチューブをクロロホルムに分散して炭素ナノチューブ分散液を得た。
[Example 1]
Single-walled carbon nanotubes synthesized by a conventional CVD method were purified by oxidation treatment with air at a temperature of 400 ° C. using a tubular reactor. The purified carbon nanotubes were further fluorinated at 40 ° C. for 30 minutes under an atmosphere of 0.1 bar of fluorine gas (F 2 ). The fluorinated carbon nanotubes were dispersed in chloroform to obtain a carbon nanotube dispersion.
［比較例１］
通常のアーク法で合成した単一壁炭素ナノチューブを管状反応器を用いて４００℃の温度で空気で酸化処理することによって精製した。精製された炭素ナノチューブを実施例１のフッ素化処理工程を省略し、蒸留水に分散して炭素ナノチューブ分散液を得た。
[Comparative Example 1]
The single-walled carbon nanotubes synthesized by the conventional arc method were purified by oxidation treatment with air at 400 ° C. using a tubular reactor. The purified carbon nanotubes were dispersed in distilled water by omitting the fluorination treatment step of Example 1 to obtain a carbon nanotube dispersion.
［比較例２］
蒸留水に５００Ｗの超音波を３０分間加えたことを除いては、比較例１と同様な方法で炭素ナノチューブ分散液を得た。
[Comparative Example 2]
A carbon nanotube dispersion was obtained in the same manner as in Comparative Example 1, except that 500 W of ultrasonic waves was applied to distilled water for 30 minutes.
［実施例２］
実施例１に従ってフッ素化処理された炭素ナノチューブを０．０１重量％のドデシルベンゼン硫酸ナトリウム水溶液に分散し、これに５００Ｗの超音波を３０分間加えて炭素ナノチューブ分散液を得た。
[Example 2]
The fluorinated carbon nanotubes according to Example 1 were dispersed in a 0.01% by weight aqueous solution of sodium dodecylbenzene sulfate, and 500 W ultrasonic waves were applied thereto for 30 minutes to obtain a carbon nanotube dispersion.
［実施例３］
ドデシルベンゼン硫酸ナトリウム水溶液の代わりに、カルボキシルメチルセルロース水溶液０．１重量％を用いたことを除いては、前記実施例２と同様な方法で炭素ナノチューブ分散液を得た。
[Example 3]
A carbon nanotube dispersion was obtained in the same manner as in Example 2, except that 0.1% by weight of an aqueous solution of carboxymethyl cellulose was used instead of the aqueous solution of sodium dodecylbenzene sulfate.
［比較例３］
フッ素化処理された炭素ナノチューブの代わりに、フッ素化処理されていない炭素ナノチューブを用いたことを除いては、前記実施例２と同様な方法で炭素ナノチューブ分散液を得た。
[Comparative Example 3]
A carbon nanotube dispersion was obtained in the same manner as in Example 2, except that a non-fluorinated carbon nanotube was used instead of the fluorinated carbon nanotube.
［実施例４］
単一壁炭素ナノチューブおよび蒸留水の代わりに、それぞれ多重壁炭素ナノチューブおよびイソプロピルアルコールを用いたことを除いては、前記実施例１と同様な方法で炭素ナノチューブ分散液を得た。
[Example 4]
A carbon nanotube dispersion was obtained in the same manner as in Example 1, except that the single-walled carbon nanotube and isopropyl alcohol were used instead of the single-walled carbon nanotube and distilled water, respectively.
［実験例１］炭素ナノチューブ分散液の粒子サイズ分布
前記比較例１〜３および実施例１〜３で得られた炭素ナノチューブ分散液の粒子サイズ分布を粒度分析計（ＥＬＳ−８０００；大塚電子株式会社製）を用いて測定した後、その結果をそれぞれ図２〜７に示す。図２〜７において、横軸は測定された炭素ナノチューブまたは炭素ナノチューブ束の直径を示し、縦軸は相対分布度を示す。
Experimental Example 1 Particle Size Distribution of Carbon Nanotube Dispersion The particle size distribution of the carbon nanotube dispersions obtained in Comparative Examples 1 to 3 and Examples 1 to 3 was measured using a particle size analyzer (ELS-8000; Otsuka Electronics Co., Ltd.). The results are shown in FIGS. 2 to 7, respectively. 2 to 7, the horizontal axis indicates the measured diameter of the carbon nanotube or the carbon nanotube bundle, and the vertical axis indicates the relative distribution.
図２は、前記比較例１に従って、フッ素化処理なしに精製工程のみを行うことによって得られた炭素ナノチューブ分散液の粒子サイズ分布を示す図であって、炭素ナノチューブが１００〜４，５００ｎｍの広範囲なサイズ範囲で分散されていることが分かる。 FIG. 2 is a diagram showing a particle size distribution of a carbon nanotube dispersion obtained by performing only a purification step without a fluorination treatment according to Comparative Example 1, wherein the carbon nanotubes have a wide range of 100 to 4,500 nm. It can be seen that they are dispersed in a wide range of sizes.
図３は、前記比較例２に従って、フッ素化処理なしに精製および超音波処理を行うことによって得られた炭素ナノチューブ分散液の粒子サイズ分布を示す図であって、炭素ナノチューブが１００〜１，０００ｎｍと依然として広範囲なサイズ範囲で分散されていることが分かる。 FIG. 3 is a diagram showing a particle size distribution of a carbon nanotube dispersion obtained by performing purification and ultrasonic treatment without fluorination treatment according to Comparative Example 2, wherein the carbon nanotubes have a particle size of 100 to 1,000 nm. It can be seen that they are still distributed over a wide size range.
図４は、前記比較例３に従って、フッ素化処理なしに精製、界面活性剤および超音波処理を行うことによって得られた炭素ナノチューブ分散液の粒子サイズ分布を示す図であって、炭素ナノチューブが単一壁炭素ナノチューブの場合よりも大きい１０〜１５ｎｍのサイズ範囲で分散されていることが分かる。 FIG. 4 is a diagram showing the particle size distribution of a carbon nanotube dispersion obtained by performing purification, surfactant and ultrasonic treatment without fluorination treatment according to Comparative Example 3, wherein the carbon nanotubes are single It can be seen that the particles are dispersed in a size range of 10 to 15 nm, which is larger than that of the single-walled carbon nanotube.
図５は、前記実施例１に従って、精製およびフッ素化処理を行うことによって得られた炭素ナノチューブ分散液の粒子サイズ分布を示す図であって、炭素ナノチューブが１〜２．５ｎｍのサイズ範囲で分散されていることが分かる。 FIG. 5 is a diagram showing a particle size distribution of a carbon nanotube dispersion obtained by performing purification and fluorination treatment according to Example 1, wherein carbon nanotubes are dispersed in a size range of 1 to 2.5 nm. You can see that it is done.
図６は、前記実施例２に従って、精製、フッ素化処理、界面活性剤および超音波処理を行うことによって得られた炭素ナノチューブ分散液の粒子サイズ分布を示す図であって、炭素ナノチューブが１〜３ｎｍのサイズ範囲で分散されていることが分かる。 FIG. 6 is a diagram showing a particle size distribution of a carbon nanotube dispersion obtained by performing purification, fluorination treatment, surfactant, and ultrasonic treatment in accordance with Example 2, wherein the carbon nanotubes are 1 to 3. It can be seen that the particles are dispersed in a size range of 3 nm.
図７は、前記実施例３に従って、精製、フッ素化処理、水溶性高分子および超音波処理を行うことによって得られた炭素ナノチューブ分散液の粒子サイズ分布を示す図であって、炭素ナノチューブが１．７〜３ｎｍのサイズ範囲で分散されていることが分かる。 FIG. 7 is a diagram showing a particle size distribution of a carbon nanotube dispersion obtained by performing purification, fluorination treatment, water-soluble polymer, and ultrasonic treatment according to Example 3, wherein It can be seen that the particles are dispersed in a size range of 0.7 to 3 nm.
このように、フッ素化処理された炭素ナノチューブは単一壁炭素ナノチューブの直径に相応する３ｎｍ以下の均一な粒子サイズ範囲で分散できる。 Thus, the fluorinated carbon nanotubes can be dispersed in a uniform particle size range of 3 nm or less corresponding to the diameter of the single-walled carbon nanotube.
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| US7682590B2 (en) | 2003-11-27 | 2010-03-23 | National Institute Of Advanced Industrial Science And Technology | Carbon nanotube dispersed polar organic solvent and method for producing the same |
| WO2010074000A1 (en) * | 2008-12-24 | 2010-07-01 | 国立大学法人東北大学 | Dispersion of carbon material and process for producing same |
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2004
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Also Published As
| Publication number | Publication date |
|---|---|
| JP3831387B2 (en) | 2006-10-11 |
| KR20040103325A (en) | 2004-12-08 |
| KR100657351B1 (en) | 2006-12-14 |
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