JP2017137229A - 窒素含有多孔性炭素材料及びそのコンデンサと製造方法 - Google Patents

窒素含有多孔性炭素材料及びそのコンデンサと製造方法 Download PDF

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Publication number
JP2017137229A
JP2017137229A JP2016131365A JP2016131365A JP2017137229A JP 2017137229 A JP2017137229 A JP 2017137229A JP 2016131365 A JP2016131365 A JP 2016131365A JP 2016131365 A JP2016131365 A JP 2016131365A JP 2017137229 A JP2017137229 A JP 2017137229A
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Prior art keywords
nitrogen
porous carbon
containing porous
carbon material
plate
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JP2016131365A
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Inventor
光哲 李
Kwang-Chul Lee
光哲 李
泊彦 廖
Po-Yen Liao
泊彦 廖
志偉 彭
Jr-Wei Peng
志偉 彭
群賢 蔡
Chun Hsien Tsai
群賢 蔡
群栄 蔡
Chun Jung Tsai
群栄 蔡
庭鵑 李
Ting Chuan Lee
庭鵑 李
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Taiwan Carbon Nano Technology Corp
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Taiwan Carbon Nano Technology Corp
Taiwan Carbon Nanotube Co Ltd
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Publication of JP2017137229A publication Critical patent/JP2017137229A/ja
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    • H—ELECTRICITY
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Abstract

【課題】従来の、比表面積が最も好ましい値に達すると、その導電、伝熱、酸化還元等の性質が一定の値に達し、それ以上向上させ難いという多孔質炭素材料の性質ををより向上させ、応用において更なる優位性を有する方法の提供。
【解決手段】まず、炭素材料と、高分子材料と、窒素を含む改質材料と、を混合して予備成形体Ｓ１を形成し、前記予備成形体に対して成形加工を行って成形体Ｓ２を得て、最後に、高温焼結を行い、一部分の前記高分子材料が分解して除去され、もう一部分の前記高分子材料と前記炭素材料とが共に、複数の孔隙を含む骨格構造を形成し、前記窒素を前記骨格構造に付着させて窒素含有官能基を形成する、窒素含有多孔性炭素材料Ｓ３。また、窒素含有多孔性炭素材料を第一窒素含有多孔性炭素板と第二窒素含有多孔性炭素板とに形成し、且つこれ等を海中に設置することで、海水を用いる蓄電コンデンサを形成することができる。
【選択図】図１

Description

本発明は、多孔性炭素材料、特に、窒素含有多孔性炭素材料及びそのコンデンサと製造方法に関するものである。
多孔性炭素材料とは、異なる大きさの孔径を有する炭素材料であって、その孔径の大きさは、分子レベルに相当する大きさを有するナノクラスの孔径から微生物の増殖及び活動に適するマイクロクラスの孔径までの範囲があり、且つ多孔性炭素材料は、耐熱、耐酸、耐アルカリ、導電及び伝熱性等といった一連の利点を有するため、気体や液体の精製、水処理、空気の浄化、触媒材料、電子エネルギー材料、生物工学材料等の方面で、幅広く応用されている。
多孔性炭素材料として、例えば、特許文献１のように、複数の大細孔と、複数の中細孔と、複数の微細孔とを包含し、各前記大細孔の孔径が５０ナノメートルより大きく、各前記中細孔の孔径が２〜５０ナノメートル、各前記微細孔が２ナノメートルより小さく、これ等大細孔の細孔体積の分布比率が１０〜２５％、これ等中細孔の細孔体積の分布比率が２０〜８０％、これ等微細孔の細孔体積の分布比率が０．０１〜２０％である多孔性炭素素材が掲示されている。これ等大細孔、これ等中細孔及びこれ等微細孔の細孔体積の分布比率を調整することで、比表面積を最も好ましい値にさせることができ、前記多孔性炭素材料の導電、伝熱、酸化還元等の性質を向上させることができる。
しかし、比表面積が最も好ましい値に達すると、その導電、伝熱、酸化還元等の性質が一定の値に達するが、それ以上向上させることができないため、どのようにして、多孔性炭素材料の性質をより向上させ、応用において更なる優位性を有するかが、当該業者における課題となっている。
アメリカ特許公開第２０１４/０１１８８８４号
本発明の主な目的は、従来の多孔質炭素材料の性質をこれ以上向上させ難いという問題を解決することにある。
上述した目的を達成するため、本発明は、
重量パーセントが３０％から８５％に介する炭素材料と、重量パーセントが１０％から６０％に介する高分子材料と、重量パーセントが３％から４０％に介し、窒素を含み、且つアミン、アミド、含窒素複素環有機化合物及びアンモニウム塩からなる群のいずれかである改質材料と、を混合して予備成形体を形成する工程Ｓ１と、
前記予備成形体に対して成形加工を行って成形体を得る工程Ｓ２と、
前記成形体に対して高温焼結を行い、一部分の前記高分子材料が分解して除去され、もう一部分の前記高分子材料と前記炭素材料とが共に、複数の孔隙を含む骨格構造を形成し、前記改質材料にある前記窒素を前記骨格構造に付着させて窒素含有官能基を形成し、窒素含有多孔性炭素材料を得る工程Ｓ３と、
を包括する窒素含有多孔性炭素材料の製造方法を提供している。
また、上述した目的を達成するため、本発明は、上述した方法で製造し、前記骨格構造を含み、大部分が炭素から構成してこれ等孔隙及び前記骨格構造が結合する前記窒素含有官能基を包含する窒素含有多孔性炭素材料をさらに提供している。
また、上述した目的を達成するため、本発明は、第一窒素含有多孔性炭素板と、前記第一窒素含有多孔性炭素板と間隔を置いて設置する第二窒素含有多孔性炭素板と、前記第一窒素含有多孔性炭素板と接触する第一コレクタ板と、前記第二窒素含有多孔性炭素板と接触する第二コレクタ板とを包括し、前記第一窒素含有多孔性炭素板、前記第二窒素含有多孔性炭素板、前記第一コレクタ板及び前記第二コレクタ板を海中に設置し、且つ前記第一窒素含有多孔性炭素板及び前記第二窒素含有多孔性炭素板を上述した方法で製造し、海中の塩化ナトリウムがナトリウムイオンと塩素イオンとに解離し、それぞれ前記第一窒素含有多孔性炭素板及び前記第二窒素含有多孔性炭素板に入り込んで蓄電する、海水を用いる蓄電コンデンサをさらにまた提供している。
このことから、本発明は、以下のような特徴を有している。
第一に、高温焼結を行う際、一部分の前記高分子材料が分解して除去され、もう一部分の前記高分子材料と前記炭素材料とが共に、前記骨格構造及びこれ等孔隙を形成しており、前記改質材料が高温によって形成する前記窒素含有官能基を合わせることで、前記窒素含有多孔性炭素材料の導電、伝熱、酸化還元、イオン酸化還元、触媒効率等といった性質をさらに向上させることができ、前記窒素含有多孔性炭素材料が応用において更なる優位性を有することができる。
第二に、従来の蓄電コンデンサは、電極がバルク材でないため、金属コレクタ板に塗布し層状或いは板状の構造に形成して使用する必要があり、また、このような電極は、厚さを増やすことが困難で、大きい体積の電極が必要な場合、電極の面積を増やすことしかできず、このとき、金属コレクタ板の面積もこれに相応して増やす必要があるが、これに対して、本発明の方法で得た窒素含有多孔性炭素材料は、剛性を有するバルク材に属し、蓄電コンデンサを用いて電極とした際、厚さを増やすことにより大きな体積に達することで、前記第一コレクタ板及び前記第二コレクタ板の使用面積を低減し、材料の使用を削減することができるため、金属コレクタ板の使用及びコストを大幅に減らすことができる。
第三に、前記第一窒素含有多孔性炭素板及び前記第二窒素含有多孔性炭素板が有する窒素含有官能基によって、一定量の疑似容量を得て蓄電能力を向上させることができる。
本発明に係る窒素含有多孔性炭素材料の製造を示すフローチャートである。 本発明に係る第一実施例の応用を示す局部断面図である。 本発明に係る第二実施例の応用を示す模式図である。
本発明の詳細な説明及び技術的内容について、図面を参照しつつ以下において説明する。
図１を参照すると、本発明は、窒素含有多孔性炭素材料及びそのコンデンサと製造方法であって、その製造方法は、以下の工程を包括している。
まず、工程Ｓ１は、炭素材料と、高分子材料と、改質材料と、を混合して予備成形体を形成しており、前記炭素素材は、カーボンブラック、炭素繊維、カーボンナノチューブ、気相成長炭素繊維、活性炭素、グラファイト、グラフェン、中空カーボン、ソフトカーボン、ハードカーボン或いはこれ等の組合せとすることができ、前記高分子材料は、フェノール樹脂（Ｐｈｅｎｏｌ ｆｏｒｍａｌｄｅｈｙｄｅ ｒｅｓｉｎ）、エポキシ樹脂（Ｅｐｏｘｙ）、ポリアクリロニトリル（Ｐｏｌｙａｃｒｙｌｏｎｉｔｒｉｌｅ，ＰＡＮ）、フラン樹脂（Ｆｕｒａｎ ｒｅｓｉｎ）、ポリビニルアルコール（Ｐｏｌｙｖｉｎｙｌ ａｌｃｏｈｏｌ，ＰＶＡ）、ポリ塩化ビニル（Ｐｏｌｙｖｉｎｙｌ ｃｈｌｏｒｉｄｅ，ＰＶＣ）、セルロース（Ｃｅｌｌｕｌｏｓｅ）、ポリフッ化ビニリデン（Ｐｏｌｙｖｉｎｙｌｉｄｅｎｅ ｆｌｕｏｒｉｄｅ，ＰＶＤＦ）、ポリテトラフルオロエチレン（Ｐｏｌｙｔｅｔｒａｆｌｕｏｒｏｅｔｈｅｎｅ，ＰＴＦＥ）、フッ素化エチレンプロピレン共重合体（Ｆｌｕｏｒｉｎａｔｅｄ ｅｔｈｙｌｅｎｅ ｐｒｏｐｙｌｅｎｅ，ＦＥＰ）或いはこれ等の組合せ等とすることができ、前記改質材料は、アミン、アミド、含窒素複素環有機化合物及びアンモニウム塩等とすることができ、且つ前記改質材料は、窒素を包含し、そのうち、前記アミンの一般式は、Ｒ１−ＮＨ２或いはＮＨ２−Ｒ１−ＮＨ２であって、Ｒ１は、例えば、ポリピルアミン、イソプロピルアミン、ヘキシルアミン、オクチルアミン、ドデシルアミン、３−メチル−２−アンモニアペンタン、エチレンジアミン等のＣ３−Ｃ２４アルキル基とすることができ、また、Ｒ１は、アニリン、トルイジン、ナフチルアミン、ベンジジン、ビフェニルジアミン、フェニレンジアミン、トリレンジアミン、２，６−トルエンジアミン等の芳香族基とすることもでき、前記アミドの一般式は、Ｒ２−ＣＯＮＨ２であって、そのうち、Ｒ２は、Ｃ１−Ｃ１８アルキル基、シクロアルキル基、又は例えば、フェニル基、ナフチル基の芳香族基とすることができ、また、Ｒ２は、アミノ基とすることもでき、前記アミドは、アセトアミド、尿素、アセトアニリド等とすることができ、前記含窒素複素環有機化合物は、５員複素環或いは６員複素環とすることができ、５員複素環の実例として、ピロリジン、ピロールがあり、６員複素環の実例として、ピリジン、ピペリジン、４−アミノ基−２−オキシピリジン、２，４−ジオキシピリミジン、メラミン、５−メチル基−２，４−ジオキシピリミジンがあり、前記アンモニア塩の一般式は、ＮＨ４ＣＯＯ−Ｒ３であって、そのうち、Ｒ３は、炭酸水素アンモニウムといったヒドロキシル基やカルバミン酸アンモニウムといったアミノ基、又は、炭酸アンモニウム、酢酸アンモニウムといった水素或いはメチル基に直接代えることもでき、また、Ｒ３は、炭酸アンモニウムといったアンモニア基とすることもできる。
また、前記予備成形体において、前記炭素材料の重量パーセントは３０％から８５％に介し、前記高分子材料の重量パーセントは１０％から６０％に介し、前記改質材料の重量パーセントは３％から４０％に介している。
次に、工程Ｓ２は、前記予備成形体に対して成形加工を行って成形体を得ており、本実施例において、前記成形加工は、前記予備成形体を１００℃から２２０℃の間に介する受熱温度と、５Ｋｇｆ／ｃｍ２から２００Ｋｇｆ／ｃｍ２の間に介する成形圧力とに置き、前記受熱温度及び前記成形圧力により、前記予備成形体の密度及び立体構造を調整し、さらにバルク状の前記成形体を形成している。また、本実施例において、前記成形加工は、熱プレス加工とすることができ、つまり、前記受熱温度及び前記成形圧力を同時に与えることができるが、本発明はこれに限定せず、例えば、先に前記予備成形体に対して前記受熱温度を与え、その後前記成形圧力を与える成形プレス加工とすることもできる。
次に、工程Ｓ３は、前記成形体に対して高温焼結を行い、一部分の前記高分子材料が分解して除去され、もう一部分の前記高分子材料と前記炭素材料とが共に、複数の孔隙を含む骨格構造を形成し、前記改質材料にある前記窒素を前記骨格構造に付着させて窒素含有官能基を形成し、窒素含有多孔性炭素材料を得ている。本実施例において、前記高温焼結が行われると、もう一部分の前記高分子材料がバインダ（Ｂｉｎｄｅｒ）の役目をし、前記炭素材料を三次元立体網目状に呈する前記骨格構造に焼結し、即ち、前記骨格構造の大部分は、炭素から構成している。本実施例の前記高温焼結は、前記成形体を還元雰囲気中に置いており、前記還元雰囲気は、アルゴンガス或いは窒素ガス等とすることができ、４００℃から１２００℃の間に介する加熱温度に置かれることで、前記高分子材料が前記成形体中で熱分解し、前記窒素含有多孔性炭素材料は、１０％から８５％の間に介する孔隙率を有し、これ等孔隙の形成によって前記炭素材料の表面積及び内部空間が増加すると共に、前記窒素含有官能基を形成することにより、前記窒素含有多孔性炭素材料の導電、伝熱、酸化還元、イオン酸化還元、触媒効率等といった性質をさらに向上させることができ、前記窒素含有多孔性炭素材料が応用において更なる優位性を有することができる。
また、前記高温焼結の過程において、前記炭素材料間に付着する外部炭素材料をさらに発生することができ、前記外部炭素材料は、恐らく、前記高分子材料或いは前記改質材料が熱分解した後に前記炭素材料間に残ったものや新たに加えた炭素含有雰囲気によって提供されたものであることから、最終的に得られた前記窒素含有多孔性炭素材料における前記炭素材料の重量パーセントは最初に加えた時より高く、導電性に優れている。
続いて、図２及び図３を参照すると、海水を用いる蓄電コンデンサであって、第一窒素含有多孔性炭素板１０と、第二窒素含有多孔性炭素板２０と、第一コレクタ板４０と、第二コレクタ板５０と、海水３０とを包括し、前記第一窒素含有多孔性炭素板１０は前記第一コレクタ板４０と接触し、前記第二窒素含有多孔性炭素板２０は前記第二コレクタ板５０と接触し、且つ前記第一窒素含有多孔性炭素板１０及び前記第二窒素含有多孔性炭素板２０は上述した方法で製造されると共に、電解質として用いられる前記海水３０の中で互いに間隔を置いて設置し、電源を接続すると、前記海水３０中にある塩化ナトリウムがナトリウムイオンと塩素イオンとに解離し、それぞれ前記第一窒素含有多孔性炭素板１０及び前記第二窒素含有多孔性炭素板２０に入り込んで蓄電している。
図２のように、本発明に係る第一実施例は、前記第一コレクタ板４０及び前記第二コレクタ５０が前記第一窒素含有多孔性炭素板１０と前記第二窒素含有多孔性炭素板２０とにそれぞれ設置しており、図３のように、本発明に係る第二実施例は、前記第一コレクタ板４０が前記第二窒素含有多孔性炭素板２０から離れた前記第一窒素含有多孔性炭素板１０の一方に設置し、前記第二コレクタ板５０が前記第一窒素含有多孔性炭素板１０から離れた前記第二窒素含有多孔性炭素板２０の一方に設置しているが、設置方法を限定するものではない。
前記第一窒素含有多孔性炭素板１０及び前記第二窒素含有多孔性炭素板２０をコンデンサの電極として使用することから、従来のコンデンサにある分離膜が使用されなくなり、コンデンサの製造コストが低減され、使用電圧が向上する上、長時間エネルギーを蓄積することが可能となり、さらに、前記第一窒素含有多孔性炭素板１０及び前記第二窒素含有多孔性炭素板２０が前記窒素含有官能基を有することから、一定量の疑似容量を得て蓄電能力を向上させることができる。また、本発明の方法で得た窒素含有多孔性炭素材料は、剛性を有するバルク材に属し、これに対して、周知技術の電極は、板状で積層構造であることから、電極が同じ体積という条件下において、本発明は、前記第一窒素含有多孔性炭素板１０及び前記第二窒素含有多孔性炭素板２０の厚さを増やすことにより大きな体積に達することで、前記第一コレクタ板４０及び前記第二コレクタ５０の使用面積を低減し、材料の使用を減らすため、金属コレクタ板の使用及びコストを大幅に減らすことができる。
以上のことから、本発明は、以下のような特徴を有している。
第一に、高温焼結を行う際、一部分の前記高分子材料が分解して除去され、もう一部分の前記高分子材料と前記炭素材料とが共に、前記骨格構造及びこれ等孔隙を形成しており、前記改質材料が高温によって形成する前記窒素含有官能基を合わせることで、前記窒素含有多孔性炭素材料の導電、伝熱、酸化還元、イオン酸化還元、触媒効率等といった性質をさらに向上させることができ、前記窒素含有多孔性炭素材料が応用において更なる優位性を有することができる。
第二に、従来の蓄電コンデンサは、電極がバルク材でないため、金属コレクタ板に塗布し層状或いは板状の構造に形成して使用する必要があり、また、このような電極は、厚さを増やすことが困難で、大きい体積の電極が必要な場合、電極の面積を増やすことしかできず、このとき、金属コレクタ板の面積もこれに相応して増やす必要があるが、これに対して、本発明の方法で得た窒素含有多孔性炭素材料は、剛性を有するバルク材に属し、蓄電コンデンサを用いて電極とした際、厚さを増やすことにより大きな体積に達するため、金属コレクタ板の使用及びコストを大幅に減らすことができる。
第三に、前記第一窒素含有多孔性炭素板及び前記第二窒素含有多孔性炭素板が有する窒素含有官能基によって、一定量の疑似容量を得て蓄電能力を向上させることができる。
以上において、本発明に係る詳細な説明を行ったが、上述したものは、本発明に係る好ましい実施例に過ぎず、本発明に係る実施の範囲を限定するものではなく、本発明に係る請求の範囲に基づいて行われたいずれの変更及び修正は、本発明に係る請求の範囲に属するものである。
１０ 第一窒素含有多孔性炭素板
２０ 第二窒素含有多孔性炭素板
３０ 海水
４０ 第一コレクタ板
４０１ 第二コレクタ板
Ｓ１〜Ｓ３ 工程

Claims (13)

  1. 重量パーセントが３０％から８５％に介する炭素材料と、重量パーセントが１０％から６０％に介する高分子材料と、重量パーセントが３％から４０％に介し、窒素を含み、且つアミン、アミド、含窒素複素環有機化合物及びアンモニウム塩からなる群のいずれかである改質材料と、を混合して予備成形体を形成する工程Ｓ１と、
    前記予備成形体に対して成形加工を行って成形体を得る工程Ｓ２と、
    前記成形体に対して高温焼結を行い、一部分の前記高分子材料が分解して除去され、もう一部分の前記高分子材料と前記炭素材料とが共に、複数の孔隙を含む骨格構造を形成し、前記改質材料にある前記窒素を前記骨格構造に付着させて窒素含有官能基を形成し、窒素含有多孔性炭素材料を得る工程Ｓ３と、
    を包括することを特徴とする窒素含有多孔性炭素材料の製造方法。
  2. 前記炭素素材は、カーボンブラック、炭素繊維、カーボンナノチューブ、気相成長炭素繊維、活性炭素、グラファイト、グラフェン、中空カーボン、ソフトカーボン及びハードカーボンからなる群のいずれかであることを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  3. 前記高分子材料は、フェノール樹脂、エポキシ樹脂、ポリアクリロニトリル、フラン樹脂、ポリビニルアルコール、ポリ塩化ビニル、セルロース、ポリフッ化ビニリデン、ポリテトラフルオロエチレン及びフッ素化エチレンプロピレン共重合体からなる群のいずれかであることを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  4. 工程Ｓ２において、前記成形加工は、前記予備成形体を１００℃から２２０℃の間に介する受熱温度と、５Ｋｇｆ／ｃｍ２から１０Ｋｇｆ／ｃｍ２の間に介する成形圧力とに置くことを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  5. 工程Ｓ３において、前記高熱焼結は、前記成形体を４００℃から１２００℃の間に介する加熱温度に置くことを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  6. 工程Ｓ３において、前記窒素含有多孔性炭素材料は、１０％から８５％の間に介する孔隙率を有することを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  7. 工程Ｓ１において、前記アミンは、ポリピルアミン、イソプロピルアミン、ヘキシルアミン、オクチルアミン、ドデシルアミン、３−メチル−２−アンモニアペンタン、エチレンジアミン、アニリン、トルイジン、ナフチルアミン、ベンジジン、ビフェニルジアミン、フェニレンジアミン、トリレンジアミン及び２，６−トルエンジアミンからなる群のいずれかであることを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  8. 工程Ｓ１において、前記アミドは、アセトアミド、尿素及びアセトアニリドからなる群のいずれかであることを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  9. 工程Ｓ１において、前記含窒素複素環有機化合物は、ピロリジン、ピロール、ピリジン、ピペリジン、４−アミノ基−２−オキシピリジン、２，４−ジオキシピリミジン、メラミン及び５−メチル基−２，４−ジオキシピリミジンからなる群のいずれかであることを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  10. 工程Ｓ１において、前記アンモニア塩は、カルバミン酸アンモニウム、炭酸水素アンモニウム、酢酸アンモニウム及び炭酸アンモニウムことを特徴とする請求項１に記載の窒素含有多孔性炭素材料の製造方法。
  11. 請求項１に係る製造方法で製造した窒素含有多孔性炭素材料であって、
    大部分が炭素から構成してこれ等孔隙を含む前記骨格構造と、
    前記骨格構造と結合する前記窒素含有官能基とを包含することを特徴とする窒素含有多孔性炭素材料。
  12. 前記骨格構造は、１０％から８５％の間に介する孔隙率を有することを特徴とする請求項１１に記載の窒素含有多孔性炭素材料。
  13. 第一窒素含有多孔性炭素板と、前記第一窒素含有多孔性炭素板と間隔を置いて設置する第二窒素含有多孔性炭素板と、前記第一窒素含有多孔性炭素板と接触する第一コレクタ板と、前記第二窒素含有多孔性炭素板と接触する第二コレクタ板とを包括し、前記第一窒素含有多孔性炭素板、前記第二窒素含有多孔性炭素板、前記第一コレクタ板及び前記第二コレクタ板を海中に設置し、且つ前記第一窒素含有多孔性炭素板及び前記第二窒素含有多孔性炭素板を請求項１に係る製造方法で製造し、海中の塩化ナトリウムがナトリウムイオンと塩素イオンとに解離し、それぞれ前記第一窒素含有多孔性炭素板及び前記第二窒素含有多孔性炭素板に入り込んで蓄電することを特徴とする、海水を用いる蓄電コンデンサ。
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