JP2005314204A5 - - Google Patents

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JP2005314204A5
JP2005314204A5 JP2004236908A JP2004236908A JP2005314204A5 JP 2005314204 A5 JP2005314204 A5 JP 2005314204A5 JP 2004236908 A JP2004236908 A JP 2004236908A JP 2004236908 A JP2004236908 A JP 2004236908A JP 2005314204 A5 JP2005314204 A5 JP 2005314204A5
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上記課題を解決する本発明は、
＜１＞（１）酸化物に粉砕処理を施す工程、および（２）酸化物表面に金属を担持する工程、により得られた金属を担持した酸化物を、５００℃〜１２００℃で炭素含有化合物と接触させカーボンナノチューブを合成することを特徴とするカーボンナノチューブの製造方法。 The present invention for solving the above problems
<1> (1) A step of subjecting an oxide to pulverization, and (2) a step of supporting a metal on the surface of the oxide. A method for producing carbon nanotubes, comprising contacting carbon nanotubes to synthesize carbon nanotubes.

＜２＞酸化物の粉砕により、該酸化物の粒径分布が、１０μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上であることを特徴とする＜１＞に記載のカーボンナノチューブの製造方法。 <2> Carbon according to <1> , wherein the oxide has a particle size distribution such that the cumulative volume of particles having a particle size of 10 μm or less is 95% or more of the total volume of all particles. Nanotube manufacturing method.

＜３＞酸化物の粉砕により、該酸化物の粒径分布が、１μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上であることを特徴とする＜１＞に記載のカーボンナノチューブの製造方法。 <3> The carbon nanotube according to <1> , wherein the oxide has a particle size distribution such that the cumulative volume of particles having a particle size of 1 μm or less is 95% or more of the total volume of all particles. Manufacturing method.

＜４＞粉砕処理後の酸化物の粒径分布を実質的に維持したまま、５００℃〜１２００℃で炭素含有化合物と接触させカーボンナノチューブを合成することを特徴とする＜１＞〜＜３＞のいずれか記載のカーボンナノチューブの製造方法。 <4> Carbon nanotubes are synthesized by contacting with a carbon-containing compound at 500 ° C. to 1200 ° C. while substantially maintaining the particle size distribution of the oxide after pulverization, <1> to <3> The manufacturing method of the carbon nanotube in any one of these .

＜５＞酸化物に金属を担持し、５００℃〜１２００℃で炭素含有化合物と接触させることによりカーボンナノチューブを合成する方法において、カーボンナノチューブを合成した後でカーボンナノチューブと酸化物を含有する組成物を粉砕して、該酸化物の粒径分布が、１０μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上となるようにすることを特徴とするカーボンナノチューブの製造方法。 <5> In a method of synthesizing carbon nanotubes by supporting a metal on an oxide and bringing it into contact with a carbon-containing compound at 500 ° C. to 1200 ° C., a composition comprising carbon nanotubes and an oxide after synthesizing carbon nanotubes And the particle size distribution of the oxide is such that the cumulative volume of particles having a particle size of 10 μm or less is 95% or more of the total volume of all particles.

＜６＞該酸化物の粒径分布が、１μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上となるようにすることを特徴とする＜５＞に記載のカーボンナノチューブの製造方法。 <6> The method for producing a carbon nanotube according to <5> , wherein the particle size distribution of the oxide is such that the cumulative volume of particles of 1 μm or less is 95% or more of the total volume of all particles. .

＜７＞カーボンナノチューブと酸化物を含有する組成物の粉砕を、カーボンナノチューブと酸化物を含む組成物からカーボンナノチューブ以外の成分を除去または分離する精製工程の前、または後、またはその間に行うことを特徴とする＜５＞または＜６＞記載のカーボンナノチューブの製造方法。 <7> The pulverization of the composition containing carbon nanotubes and oxide is performed before, after, or during the purification step of removing or separating components other than carbon nanotubes from the composition containing carbon nanotubes and oxide. <5> or <6> The method for producing a carbon nanotube according to <6> .

＜８＞前記粉砕したカーボンナノチューブ含有組成物に対して、粒径分布を実質的に維持する手段を施すことを特徴とする＜５＞〜＜７＞のいずれか記載のカーボンナノチューブの製造方法。 <8> The method for producing carbon nanotubes according to any one of <5> to <7> , wherein means for substantially maintaining a particle size distribution is applied to the pulverized carbon nanotube-containing composition.

＜９＞粉砕の手段が、粒子の微粒化、凝集体の解砕または分級のうち少なくとも一つの方法により行われることを特徴とする＜１＞〜＜８＞のいずれかに記載のカーボンナノチューブの製造方法。 <9> The carbon nanotube according to any one of <1> to <8> , wherein the pulverization means is performed by at least one of particle atomization, aggregate crushing, and classification. Production method.

＜１０＞粉砕の手段が、ジェットミル法、ビーズミル法のうち少なくともどちらか一方を含むものであることを特徴とする＜１＞〜＜８＞のいずれかに記載のカーボンナノチューブの製造方法。 <10> The method for producing carbon nanotubes according to any one of <1> to <8> , wherein the pulverizing means includes at least one of a jet mill method and a bead mill method.

＜１１＞酸化物がシリカ、アルミナ、マグネシア、チタニア、ゼオライトのうち少なくとも１つを含む＜１＞〜＜１０＞のいずれかに記載のカーボンナノチューブの製造方法。 <11> The method for producing a carbon nanotube according to any one of <1> to <10> , wherein the oxide includes at least one of silica, alumina, magnesia, titania, and zeolite.

＜１２＞炭素含有化合物がメタン、エチレン、アセチレン、ベンゼン、トルエン、メタノール、エタノール、アセトン、一酸化炭素のうち少なくとも１つを含む＜１＞〜＜１１＞のいずれかに記載のカーボンナノチューブの製造方法。 <12> The carbon nanotube production according to any one of <1> to <11> , wherein the carbon-containing compound contains at least one of methane, ethylene, acetylene, benzene, toluene, methanol, ethanol, acetone, and carbon monoxide. Method.

＜１３＞＜１＞〜＜１２＞のいずれかに記載した製造方法により得られるカーボンナノチューブ含有組成物であって、カーボンナノチューブの主成分が単層カーボンナノチューブまたは２層カーボンナノチューブであることを特徴とするカーボンナノチューブ含有組成物。 <13><1> to a carbon nanotube-containing composition obtained by the production method described in any one of <12>, wherein the main component of the carbon nanotubes are single-walled carbon nanotubes or double-walled carbon nanotube And a carbon nanotube-containing composition.

＜１４＞カーボンナノチューブの総本数の５０％以上が直径１．０ｎｍ〜１．５ｎｍの単層カーボンナノチューブまたは直径１〜６ｎｍの２層カーボンナノチューブであることを特徴とする＜１３＞記載のカーボンナノチューブ含有組成物。 <14>, wherein the at least 50% of the total number of carbon nanotubes are double-walled carbon nanotubes of single-walled carbon nanotubes or diameter 1~6nm diameter 1.0Nm～1.5Nm <13> carbon nanotube according Containing composition.

＜１５＞＜１＞〜＜１２＞のいずれかに記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、＜１３＞または＜１４＞記載のカーボンナノチューブ含有組成物を含む電子放出材料。 <15> A carbon nanotube-containing composition obtained by the production method according to any one of <1> to <12> , or an electron emission material comprising the carbon nanotube-containing composition according to <13> or <14> .

＜１６＞＜１＞〜＜１２＞のいずれかに記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、＜１３＞または＜１４＞記載のカーボンナノチューブ含有組成物を含む電池電極材料。 <16> A carbon electrode-containing composition obtained by the production method according to any one of <1> to <12> , or a battery electrode material comprising the carbon nanotube-containing composition according to <13> or <14> .

＜１７＞＜１＞〜＜１２＞のいずれかに記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、＜１３＞または＜１４＞記載のカーボンナノチューブ含有組成物を含む樹脂組成物。
＜１８＞＜１＞〜＜１２＞のいずれかに記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、＜１３＞または＜１４＞記載のカーボンナノチューブ含有組成物を含むコーティング用材料。 <17> A carbon nanotube-containing composition obtained by the production method described in any one of <1> to <12> , or a resin composition containing the carbon nanotube-containing composition described in <13> or <14> .
<18> A carbon nanotube-containing composition obtained by the production method described in any one of <1> to <12> , or a coating material comprising the carbon nanotube-containing composition described in <13> or <14> .

Claims (18)

（１）酸化物に粉砕処理を施す工程、および（２）酸化物表面に金属を担持する工程、により得られた金属を担持した酸化物を、５００℃〜１２００℃で炭素含有化合物と接触させカーボンナノチューブを合成することを特徴とするカーボンナノチューブの製造方法。The oxide obtained by carrying the metal obtained by (1) the step of pulverizing the oxide and (2) the step of carrying the metal on the oxide surface is brought into contact with the carbon-containing compound at 500 ° C. to 1200 ° C. A method for producing carbon nanotubes, comprising synthesizing carbon nanotubes. 酸化物の粉砕により、該酸化物の粒径分布が、１０μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上であることを特徴とする請求項１に記載のカーボンナノチューブの製造方法。 The carbon nanotube production according to claim 1 , wherein the oxide has a particle size distribution such that the cumulative volume of particles having a particle size of 10 µm or less is 95% or more of the total volume of all particles. Method. 酸化物の粉砕により、該酸化物の粒径分布が、１μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上であることを特徴とする請求項１に記載のカーボンナノチューブの製造方法。 The method for producing carbon nanotubes according to claim 1 , wherein the oxide has a particle size distribution such that the cumulative volume of particles having a particle size of 1 µm or less is 95% or more of the total volume of all particles. . 粉砕処理後の酸化物の粒径分布を実質的に維持したまま、５００℃〜１２００℃で炭素含有化合物と接触させカーボンナノチューブを合成することを特徴とする請求項１〜３のいずれかに記載のカーボンナノチューブの製造方法。 While substantially maintaining the particle size distribution of oxide after pulverization treatment, according to any one of claims 1 to 3, wherein the synthesis of carbon nanotubes are contacted with a carbon-containing compound at 500 ° C. to 1200 ° C. Carbon nanotube manufacturing method. 酸化物に金属を担持し、５００℃〜１２００℃で炭素含有化合物と接触させることによりカーボンナノチューブを合成する方法において、カーボンナノチューブを合成した後でカーボンナノチューブと酸化物を含有する組成物を粉砕して、該酸化物の粒径分布が、１０μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上となるようにすることを特徴とするカーボンナノチューブの製造方法。 In a method of synthesizing a carbon nanotube by supporting a metal on an oxide and contacting with a carbon-containing compound at 500 ° C. to 1200 ° C., the composition containing the carbon nanotube and the oxide is pulverized after synthesizing the carbon nanotube. A method for producing carbon nanotubes, wherein the particle size distribution of the oxide is such that the cumulative volume of particles of 10 μm or less is 95% or more of the total volume of all particles. 該酸化物の粒径分布が、１μｍ以下の粒子の累積体積が全粒子の総体積の９５％以上となるようにすることを特徴とする請求項５に記載のカーボンナノチューブの製造方法。 6. The method for producing carbon nanotubes according to claim 5 , wherein the particle size distribution of the oxide is such that the cumulative volume of particles of 1 μm or less is 95% or more of the total volume of all particles. カーボンナノチューブと酸化物を含有する組成物の粉砕を、カーボンナノチューブと酸化物を含む組成物からカーボンナノチューブ以外の成分を除去または分離する精製工程の前、または後、またはその間に行うことを特徴とする請求項５または６に記載のカーボンナノチューブの製造方法。 The composition containing carbon nanotubes and oxides is pulverized before, after, or during a purification step of removing or separating components other than carbon nanotubes from the composition containing carbon nanotubes and oxides. The manufacturing method of the carbon nanotube of Claim 5 or 6 . 前記粉砕したカーボンナノチューブ含有組成物に対して、粒径分布を実質的に維持する手段を施すことを特徴とする請求項５〜７のいずれか１項に記載のカーボンナノチューブの製造方法。 The method for producing carbon nanotubes according to any one of claims 5 to 7 , wherein means for substantially maintaining a particle size distribution is applied to the pulverized carbon nanotube-containing composition. 粉砕の手段が、粒子の微粒化、凝集体の解砕または分級のうち少なくとも一つの方法により行われることを特徴とする請求項１〜８のいずれか１項に記載のカーボンナノチューブの製造方法。 The method for producing carbon nanotubes according to any one of claims 1 to 8 , wherein the pulverizing means is performed by at least one of atomization of particles, crushing of aggregates, and classification. 粉砕の手段が、ジェットミル法、ビーズミル法のうち少なくともどちらか一方を含むものであることを特徴とする請求項１〜９のいずれか１項に記載のカーボンナノチューブの製造方法。 The method for producing carbon nanotubes according to any one of claims 1 to 9 , wherein the pulverizing means includes at least one of a jet mill method and a bead mill method. 酸化物がシリカ、アルミナ、マグネシア、チタニア、ゼオライトのうち少なくとも１つを含む請求項１〜１０のいずれか１項に記載のカーボンナノチューブの製造方法。 The method for producing a carbon nanotube according to any one of claims 1 to 10 , wherein the oxide contains at least one of silica, alumina, magnesia, titania, and zeolite. 炭素含有化合物がメタン、エチレン、アセチレン、ベンゼン、トルエン、メタノール、エタノール、アセトン、一酸化炭素のうち少なくとも１つを含む請求項１〜１１のいずれか１項に記載のカーボンナノチューブの製造方法。 The carbon nanotube production method according to any one of claims 1 to 11 , wherein the carbon-containing compound contains at least one of methane, ethylene, acetylene, benzene, toluene, methanol, ethanol, acetone, and carbon monoxide. 請求項１〜１２のいずれか１項に記載した製造方法により得られるカーボンナノチューブ含有組成物であって、カーボンナノチューブの主成分が単層カーボンナノチューブまたは２層カーボンナノチューブであることを特徴とするカーボンナノチューブ含有組成物。 A carbon nanotube-containing composition obtained by the production method described in any one of claims 1 to 12 carbon, wherein the main component of the carbon nanotubes are single-walled carbon nanotubes or double-walled carbon nanotube Nanotube-containing composition. カーボンナノチューブの総本数の５０％以上が直径１．０ｎｍ〜１．５ｎｍの単層カーボンナノチューブまたは直径１〜６ｎｍの２層カーボンナノチューブであることを特徴とする請求項１３記載のカーボンナノチューブ含有組成物。 14. The carbon nanotube-containing composition according to claim 13 , wherein 50% or more of the total number of carbon nanotubes is a single-walled carbon nanotube having a diameter of 1.0 nm to 1.5 nm or a double-walled carbon nanotube having a diameter of 1 to 6 nm. . 請求項１〜１２のいずれか１項に記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、請求項１３または１４のいずれか１項に記載のカーボンナノチューブ含有組成物を含む電子放出材料。 Carbon nanotube-containing composition obtained by the production method described in any one of claims 1 to 12 or the electron-emitting material containing a carbon nanotube-containing composition according to any one of claims 13 or 14. 請求項１〜１２のいずれか１項に記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、請求項１３または１４のいずれか１項に記載のカーボンナノチューブ含有組成物を含む電池電極材料。 Carbon nanotube-containing composition obtained by the production method described in any one of claims 1 to 12 or a battery electrode material containing carbon nanotube-containing composition according to any one of claims 13 or 14. 請求項１〜１２のいずれか１項に記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、請求項１３または１４のいずれか１項に記載のカーボンナノチューブ含有組成物を含む樹脂組成物。 Carbon nanotube-containing composition obtained by the production method described in any one of claims 1 to 12 or a resin composition containing a carbon nanotube-containing composition according to any one of claims 13 or 14. 請求項１〜１２のいずれか１項に記載した製造方法により得られるカーボンナノチューブ含有組成物、あるいは、請求項１３〜１４のいずれか１項に記載のカーボンナノチューブ含有組成物を含むコーティング用材料。 Carbon nanotube-containing composition obtained by the production method described in any one of claims 1 to 12 or a coating material containing the carbon nanotube-containing composition according to any one of claims 13 to 14.
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