JP6320700B2 - 金属−炭素繊維複合体及びその製造方法、並びに炭素繊維及びその製造方法 - Google Patents
金属−炭素繊維複合体及びその製造方法、並びに炭素繊維及びその製造方法 Download PDFInfo
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims description 87
- 239000004917 carbon fiber Substances 0.000 title claims description 87
- 239000002131 composite material Substances 0.000 title claims description 55
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims description 38
- 238000004519 manufacturing process Methods 0.000 title claims description 16
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- 239000010941 cobalt Substances 0.000 claims description 17
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- 239000011159 matrix material Substances 0.000 claims description 7
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- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
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- 229910052758 niobium Inorganic materials 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
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- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
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- 238000009692 water atomization Methods 0.000 description 2
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910017816 Cu—Co Inorganic materials 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
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Description
上記第2の金属は、鉄、コバルト、ニッケル又はパラジウムからなる群から選択された2種以上の金属からなることがより好ましく、鉄とコバルトであることが、さらに好ましい。
本発明に係る金属−炭素繊維複合体は、金属と、該金属の表面から延びている、複数の炭素繊維とを備える。上記金属の形状としては、特に限定されず、例えば、粉体状、箔状又は線状のものを用いることができる。粉体状である場合、その数平均粒子径は、好ましくは、0.5〜45μmである。上記金属は、マトリックスとなる触媒活性のない第1の金属と、触媒活性のある2種以上の第2の金属とを含む、金属複合体である。上記第2の金属は、上記第1の金属の表面と内部のうち少なくとも一方に分散されているナノ微粒子である。上記ナノ微粒子は、上記第1の金属の表面と内部の双方、又は表面のみに分散されていることが望ましい。この上記ナノ微粒子は触媒として作用し、上記炭素繊維は、上記ナノ微粒子から延びている構造をとることができる。
本発明に係る金属−炭素繊維複合体の製造方法では、まず、マトリックスとなる第1の金属と、上記第1の金属の表面と内部のうち少なくとも一方に分散している、触媒活性のある2種以上の第2の金属のナノ微粒子とを含む、金属複合体を準備する工程1と、上記ナノ微粒子に加熱下で炭素源を接触させる化学気相成長法(CVD法)により、上記金属−炭素繊維複合体を生成する工程2とを備える。
(金属複合体の作製)
表1の組成の金属複合体の溶解物から、水アトマイズ法、又はガスアトマイズ法により、Cu−Fe−Co及びCu−Co等の各金属微粒子(粉体)を製造した。
4gの上記金属複合体粉を、内径26mm長さ70mmの石英セル中に投入し、内径32mm、長さ700mmのロータリー円筒形石英管を用いた、銅炭素複合CVD反応器(ロータリーキルン)により、表1の条件で金属複合体上に炭素繊維を生成し、表1に示す実施例1〜5及び比較例1〜3の金属−炭素繊維複合体を作製した。
1)SEMによる観察
実施例1〜5及び比較例1〜3の金属−炭素繊維複合体をFE−SEMによって観察した。結果を、図3〜図11及び表2に示す。実施例1〜5においては、細孔を側面に持つ炭素繊維が生成していることを観察できた。
本発明のメソ孔性炭素繊維の比表面積や、メソ孔及びマクロ孔の測定方法は、多孔質材料の同定法として使用される、N2(メソ〜マクロ孔の場合)を用いたガス吸着法による細孔分布測定法を用いる。本発明の比表面積測定と細孔分布測定は、島津製作所株式会社製の定容量式ガス吸着法測定装置BELSORP−miniを用いた。対象試料の前処理としては、80℃、2時間脱ガス処理を行った。吸着ガスとしてN2を使用した。比表面積は、BET法で算出される。メソ孔〜マクロ孔測定の場合、液体N2温度-196℃で相対圧約0.01〜0.99までの等温吸着測定を実施した。メソ孔〜マクロ孔の場合、同装置のDH解析法にて約20〜2000Åの範囲のメソ孔〜マクロ孔の細孔分布を算出した。ピーク微分細孔容積とは上記解析ソフトにて導出されるメソ孔〜マクロ孔の細孔分布のピークまたはショルダー中心値の細孔容量値のことを指す。メソ孔〜マクロ孔の細孔分布におけるピーク径とは、横軸を対数表示したその細孔分布に現れるピークやショルダー状のピーク系及びショルダーの中心値を意味する。
Claims (8)
- マトリックスとなる銅と、前記銅の内部に分散されている、鉄及びコバルトを含む2種以上の金属からなるナノ微粒子とを含む金属複合体と、
前記ナノ微粒子から延びている複数の細孔を有する炭素繊維とを備える、金属−炭素繊維複合体。 - 前記金属複合体中に、前記鉄及びコバルトを含む2種以上の金属が、0.3〜18重量%の割合で含有されている、請求項1に記載の金属−炭素繊維複合体。
- 前記細孔が、メソ孔又はマクロ孔を含む、請求項1又は2に記載の金属−炭素繊維複合体。
- 前記メソ孔又はマクロ孔の孔径が、10nm〜200nmである、請求項1〜3のいずれか1項に記載の金属−炭素繊維複合体。
- 前記細孔が、前記炭素繊維の側面と横断面の双方に存在している、請求項1〜4のいずれか1項に記載の金属−炭素繊維複合体。
- 請求項1〜5のいずれか1項に記載の金属−炭素繊維複合体の製造方法であって、
前記銅と、前記銅の内部に分散している前記鉄及びコバルトを含む2種以上の金属のナノ微粒子とを含む、金属複合体を準備する工程と、
前記ナノ微粒子に加熱下で炭素源を接触させる工程とを備える、金属−炭素繊維複合体の製造方法。 - 前記金属複合体を準備する工程が、前記銅と前記鉄及びコバルトを含む2種以上の金属に熱処理を施すことにより行われる、請求項6に記載の金属−炭素繊維複合体の製造方法。
- 請求項1〜5のいずれか1項に記載の金属−炭素繊維複合体から、酸やアルカリにより金属複合体を除去する方法、又は炭素繊維を切断した後に分級する方法により、金属複合体を単離する工程を備える、複数の細孔を有する炭素繊維の製造方法。
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