JP2021521094A - ナノ構造炭素材料を製造するための前駆体材料及び方法 - Google Patents
ナノ構造炭素材料を製造するための前駆体材料及び方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 50
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 47
- 239000002243 precursor Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 39
- 150000003839 salts Chemical class 0.000 claims abstract description 19
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 12
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000002717 carbon nanostructure Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000011852 carbon nanoparticle Substances 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000002134 carbon nanofiber Substances 0.000 claims description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Inorganic materials [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 3
- 239000003570 air Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 238000004804 winding Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 13
- 239000002184 metal Substances 0.000 abstract description 13
- 239000011435 rock Substances 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 8
- 239000004917 carbon fiber Substances 0.000 abstract description 7
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 6
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 6
- 150000004706 metal oxides Chemical class 0.000 abstract description 6
- 238000004146 energy storage Methods 0.000 abstract description 4
- 239000011149 active material Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 229910021392 nanocarbon Inorganic materials 0.000 abstract description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002482 conductive additive Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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Abstract
Description
前駆体材料(1)を、Mo、W又はNiで作られたワイヤ線(2)で包み、ワイヤ線(2)は、前駆体材料(1)のサイズに応じて、0.5mm−12mmの直径を有し、前記前駆体材料(1)に、直径5mm−6mmの導電バーA(3)の一端を固定し、ワイヤ線(2)は、導電バーA(3)に、巻回中に接続されるステップ1と、
導電バーAを有し、導電ワイヤを包む前駆体材料を、LiCl、NaCl、CaCl2又はKClの1つ又は2つ以上の混合物である溶融塩(6)が充填された、グラファイト、Mo又はWで作られた反応容器(4)の底部のセラミックディスク(5)の上に放置するステップ2と、
溶融塩の温度が350℃〜900℃であり、反応容器(4)に、導電バーA(3)と同じ材質の導電バーB(7)を接続し、導電バーA(3)は電源の負電極に接続され、導電バーB(7)は電源の正電極に接続されるステップ3と、
前駆体材料のサイズに応じて、1〜10000Aの直流電流を流れて、10min〜20h通電し、炭素ナノ構造体を生成し、溶融塩が冷却した後、溶融塩を溶解し、ナノ構造炭素材料を濾過して回収するステップ4と、を含む。
Claims (6)
- 炭素相と非炭素相とを含み、非炭素相が炭素相中に分散しており、前記非炭素相の特徴的な元素がFe、Ni、Co、Si、Na、Mg、Al、K及びCaの元素の1種又は2種以上を含み、前駆体材料中の非炭素相の特徴的な元素の質量百分率が0.1〜5%であり、前記非炭素相の特徴的な元素が単体又はその酸化物の形態で存在し、炭素相は非晶質炭素又は晶質炭素であり、非炭素相中の特徴的な元素の単体又はその酸化物の粒径が1nm〜100μmであることを特徴とするナノ構造炭素材料を製造するための前駆体材料。
- 前駆体材料(1)を、Mo、W又はNiで作られたワイヤ線(2)で包み、ワイヤ線(2)は、前駆体材料(1)のサイズに応じて、0.5mm−12mmの直径を有し、前記前駆体材料(1)に、直径5mm−6mmの導電バーA(3)の一端を固定し、ワイヤ線(2)は、導電バーA(3)に、巻回中に接続されるステップ1と、
導電バーAを有し、導電ワイヤを包む前駆体材料を、LiCl、NaCl、CaCl2又はKClの1つ又は2つ以上の混合物である溶融塩(6)が充填された、グラファイト、Mo又はWで作られた反応容器(4)の底部のセラミックディスク(5)の上に放置するステップ2と、
溶融塩の温度が350℃〜900℃であり、反応容器(4)に、導電バーA(3)と同じ材質の導電バーB(7)を接続し、導電バーA(3)は電源の負電極に接続され、導電バーB(7)は電源の正電極に接続されるステップ3と、
前駆体材料のサイズに応じて、1〜10000Aの直流電流を流れて、10min〜20h通電し、炭素ナノ構造を生成し、溶融塩が冷却した後、溶融塩を溶解し、ナノ構造炭素材料を濾過して回収するステップ4と、
を含むことを特徴とする請求項1に記載の前駆体材料を使用してナノ構造炭素材料を製造する方法。 - セラミックディスク(5)は、Al2O3、MgO又はZrO2で作られることを特徴とする請求項2に記載のナノ構造炭素材料を製造する方法。
- 導電バーB(7)と導電バーA(3)の材質は、Mo、W、Ni又はステンレスのいずれかであることを特徴とする請求項2に記載のナノ構造炭素材料を製造する方法。
- 前駆体材料の反応容器内の雰囲気が、アルゴン、空気、窒素、ヘリウムの1つ又は2つ以上の混合雰囲気であることを特徴とする請求項2に記載のナノ構造炭素材料を製造する方法。
- ステップ4で得られたナノ構造炭素材料は、1nm〜1000nmの大きさの炭素ナノ粒子と、直径1nm〜1000nmの炭素ナノ繊維と、外径1nm〜1000nmの炭素ナノチューブとを含むことを特徴とする請求項2に記載のナノ構造炭素材料を製造する方法。
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