JP6572033B2 - 水素吸蔵炭素材料 - Google Patents
水素吸蔵炭素材料 Download PDFInfo
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Description
実施例1においては、有機化合物を含み金属を含まない原料を炭素化することにより、水素吸蔵炭素材料を製造した。すなわち、フェノール樹脂製のビーズ(100μm、群栄化学工業株式会社製)を真空下で加熱して、その温度を昇温速度48℃/hで室温から800℃まで上昇させ、その後、800℃の炭素化温度で1時間保持することにより、炭素化を行った。炭素化後、自然冷却により温度を室温まで低下させた。こうして得られた内部に金属を含まない炭素材料を、実施例1に係る水素吸蔵炭素材料として使用した。実施例2においては、炭素化温度を1000℃としたこと以外は、上述の実施例1と同様にして、水素吸蔵炭素材料を製造した。
273KにてCO2吸脱着測定を行った。すなわち、上述のようにして得られた各炭素材料の比表面積、ミクロ孔容積及びウルトラミクロ孔容積を、高圧ガス吸着量測定装置(BELSORP−HP、日本ベル株式会社)を用いて測定した。
秤量した炭素材料を圧縮せずに乾いたメスシリンダーに静かに入れ、次いで、粉体層の上面を圧縮せずに注意深くならし、その体積を最小目盛単位まで読み取ることにより、当該炭素材料の嵩密度(g/cm3)を求めた。
乾式自動密度計(アキュピックII1340、マイクロメリティクス社製)及びHeガスを用い、25℃にて、ガス置換法により真密度を測定した。
まず、炭素材料の試料を、ガラス試料板の凹部に入れるとともにスライドガラスで押さえ、当該試料をその表面と基準面とが一致するように当該凹部に均一に充填した。次いで、この充填された試料の形態が崩れないように、ガラス試料板を広角X線回折試料台に固定した。そして、X線回折装置(RigakuRINT2100/PC、株式会社リガク)を用いて各試料の粉末X回折測定を実施して回折ピークを測定し、積算を5回行うことで解析対象となるX線回折データを得た。なお、X線管球への印加電圧及び電流はそれぞれ50kV及び300mAであり、サンプリング間隔は0.1°又は0.01°であり、走査速度は1°/分であり、測定角度範囲(2θ)は5〜90°であった。また、入射X線としてはCuKα線を用いた。そして、得られたX線回折図に基づき、回折角2θが18°以上、26°以下の範囲に現れる回折ピークのトップの位置を特定した。
上述の粉末X線回折で得られたX線回折データに基づいて、結晶子サイズLaに関する評価を行った。すなわち、平均La及びLa分布を、Diamond法を用いて解析した。この解析には、コンピュータにインストールされた解析用ソフトウェア(CarbonAnalyzer Dseries、藤本宏之)を用いた。解析対象データは、CuKα線をX線源としてカウンターグラファイトモノクロメータを用いて測定された炭素材料の11バンド強度に限定した。解析可能な最大網面サイズは約7nmであった。
また、上述の粉末X線回折で得られたX線回折データに基づいて、炭素構造における炭素網面の積層構造に関する評価を行った。すなわち、平均Lc、炭素網面の積層数とその分布、及び平均面間隔d002を、コンピュータにインストールされた上述の解析用ソフトウェア(CarbonAnalyzer Dseries、藤本宏之)を用いて解析した。
JIS H 7201に準拠した方法で、298Kにて、水素圧力0MPa〜11.5MPaにおける水素吸蔵量を測定した。また、こうして得られた水素圧力10MPaにおける水素吸蔵量(重量%)を、炭素材料1g当たりの水素吸蔵量(g)に換算し、得られた値を嵩密度又は真密度で除することにより、単位体積積あたりの水素吸蔵量(mg/cm3)を算出した。
炭素材料の試料を高圧NMR石英製試料管に入れた。次いで、排気・ガス導入用の配管及びバルブを取り付けた後、温度573K、最終到達圧力1×10−4torrで24時間脱気処理をした。脱気処理後の試料は減圧状態のまま速やかにプローブに設置し、水素を3.5MPaとなるまで導入して測定に供した。1H−NMR測定は高圧温度可変型プローブを装着したFT−NMR装置(Apollo Pulse NMR Spectrometer、38MHz、Tecmag社製)を用いて行った。パルス系列は90°パルス法とした。測定温度は173Kとした。なお、炭素材料の試料を高圧NMR石英製試料管の半分の充てん量としたときに増加する気体状の水素(水素ガス:試料粒子間に存在する気相水素)に起因するピーク(第一のピーク)の位置を基準(0ppm)とし、当該第一のピークに対して高磁場側にシフトしたピーク(第二のピーク)の化学シフトを評価した。芳香族環の平面上に存在する水素は芳香族環の環電流の効果により高磁場側、即ち低ppm側へシフトする。このシフト量は炭素網面構造の発達の程度に対応し、炭素網面構造が発達した炭素材料表面や細孔に吸蔵した水素は大きなシフトを示す。したがって、第二のピークは炭素材料に吸着した水素に起因すると考えられ、吸蔵サイトの構造の変化に依存してピークシフト量が変化すると考えられた。
図1には、実施例1〜3及び比較例1〜5に係る炭素材料について、炭素化温度(℃)、比表面積(m2/g)、ミクロ孔容積(cm3/g)、ウルトラミクロ孔容積(cm3/g)、及び当該ミクロ孔容積に対するウルトラミクロ孔容積の割合(%)を示す。なお、比較例3に係る炭素材料については、比表面積及び孔容積を適切に測定できなかった。その理由としては、孔サイズがCO2吸脱着測定に適さないほど小さかった可能性が考えられる。
Claims (6)
- ミクロ孔容積に対するウルトラミクロ孔容積の割合が60%以上であり、吸蔵された水素が、 1 H−NMR測定において、気体状の水素に起因する第一のピークに対する化学シフト−2ppm〜−20ppmの位置に第二のピークを示す炭素構造を有し、
前記炭素構造のa軸方向の平均結晶子サイズLaが、1.00nm以上、2.50nm以下である
ことを特徴とする水素吸蔵炭素材料。 - ミクロ孔容積に対するウルトラミクロ孔容積の割合が60%以上であり、吸蔵された水素が、 1 H−NMR測定において、気体状の水素に起因する第一のピークに対する化学シフト−2ppm〜−20ppmの位置に第二のピークを示す炭素構造を有し、
前記ミクロ孔容積が、0.19cm3/g以上、0.40cm3/g以下である
ことを特徴とする水素吸蔵炭素材料。 - ミクロ孔容積に対するウルトラミクロ孔容積の割合が60%以上であり、吸蔵された水素が、 1 H−NMR測定において、気体状の水素に起因する第一のピークに対する化学シフト−2ppm〜−20ppmの位置に第二のピークを示す炭素構造を有し、
真密度が、1.40g/cm3以上、3.00g/cm3以下である
ことを特徴とする水素吸蔵炭素材料。 - ミクロ孔容積に対するウルトラミクロ孔容積の割合が60%以上であり、吸蔵された水素が、 1 H−NMR測定において、気体状の水素に起因する第一のピークに対する化学シフト−2ppm〜−20ppmの位置に第二のピークを示す炭素構造を有し、
粉末X線回折において、ピークトップ位置が18.0°以上、25.0°以下のピーク
を示す前記炭素構造を有する
ことを特徴とする水素吸蔵炭素材料。 - 内部に金属を含まない
ことを特徴とする請求項1乃至4のいずれかに記載の水素吸蔵炭素材料。 - 請求項1乃至5のいずれかに記載の水素吸蔵炭素材料を水素吸蔵に使用する方法。
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JP2015138774A JP6572033B2 (ja) | 2015-07-10 | 2015-07-10 | 水素吸蔵炭素材料 |
EP16824215.4A EP3320968A4 (en) | 2015-07-10 | 2016-06-17 | CARBONACEOUS STORAGE SUBSTANCE OF HYDROGEN |
PCT/JP2016/068187 WO2017010235A1 (ja) | 2015-07-10 | 2016-06-17 | 水素吸蔵炭素材料 |
US15/735,777 US10392249B2 (en) | 2015-07-10 | 2016-06-17 | Hydrogen storage carbon material |
CN201680037567.3A CN107709230B (zh) | 2015-07-10 | 2016-06-17 | 储氢碳材料 |
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JP6572033B2 true JP6572033B2 (ja) | 2019-09-04 |
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JP2013112572A (ja) * | 2011-11-29 | 2013-06-10 | Nagaoka Univ Of Technology | 水素吸蔵方法及び水素吸蔵材料 |
US9597656B2 (en) * | 2012-01-11 | 2017-03-21 | William Marsh Rice University | Porous carbon materials for CO2 separation in natural gas |
US9409777B2 (en) * | 2012-02-09 | 2016-08-09 | Basf Se | Preparation of polymeric resins and carbon materials |
JP5683536B2 (ja) * | 2012-06-08 | 2015-03-11 | 株式会社豊田自動織機 | 電動圧縮機 |
KR101438433B1 (ko) * | 2012-10-09 | 2014-09-12 | 고려대학교 산학협력단 | 메조 다공성 탄소 구조체 및 그 제조방법 |
US20150291432A1 (en) * | 2012-11-16 | 2015-10-15 | Politechnika Poznanska | Production of activated carbon from tobacco leaves by simultaneous carbonization and self-activation and the activated carbon thus obtained |
WO2017040299A1 (en) * | 2015-08-28 | 2017-03-09 | Energ2 Technologies, Inc. | Novel materials with extremely durable intercalation of lithium and manufacturing methods thereof |
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