JPWO2005095274A1 - カーボンナノチューブの集合体及びその形成方法並びに生体適合性材料 - Google Patents
カーボンナノチューブの集合体及びその形成方法並びに生体適合性材料 Download PDFInfo
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- JPWO2005095274A1 JPWO2005095274A1 JP2006511819A JP2006511819A JPWO2005095274A1 JP WO2005095274 A1 JPWO2005095274 A1 JP WO2005095274A1 JP 2006511819 A JP2006511819 A JP 2006511819A JP 2006511819 A JP2006511819 A JP 2006511819A JP WO2005095274 A1 JPWO2005095274 A1 JP WO2005095274A1
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- carbon nanotube
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Abstract
Description
特許文献2には、成形品の外観が良好で、機械的強度が向上した難燃性の高い導電性熱可塑性樹脂組成物として、(A)熱可塑性樹脂20〜99.95質量%および(B)カーボンナノチューブ0.05〜20質量%からなり、(A)および(B)の合計量100質量部に対して、(C)難燃剤0.05〜30質量部およびポリフルオロオレフィン樹脂0〜2質量部を配合してなる熱可塑性樹脂組成物が開示されている。
特許文献3には、優れた力学的特性、成形性を有し、必要に応じ優れた導電性を兼ね備えたカーボン含有樹脂組成物として、構成要素[A]同士が実質的に凝集体を形成せずに絡み合いなく構成要素[B]中に均一に分散しており、構成要素[A]が組成物100重量%に対して0.01〜1.8重量%の範囲内、構成要素[C]が0.1〜55重量%の範囲内であるカーボン含有樹脂組成物が開示されている。
構成要素[A]:平均直径が1〜45nm、平均アスペクト比が5以上であるカーボンナノチューブ
構成要素[B]:樹脂
構成要素[C]:充填剤
これら従来技術は、いずれもマトリックスに、カーボンナノチューブを添加することで電気的性質、熱的性質、機械的性質を向上させることに関するものである。カーボンナノチューブの添加はあくまでマトリクスの物性向上を目的としたもので、カーボンナノチューブの優れた物性を、マクロな状態で使用可能なものにしたものではない。本発明者等はカーボンナノチューブの物性を最大限活用するためには純粋なカーボンナノチューブのみからなる集合体を構築することが最も望ましいと考えた。そこで、上記従来公報などで実施されていないカーボンナノチューブの集合体を得ることを課題としている。
本発明のカーボンナノチューブの集合体はマトリックスとしての樹脂やバインダーなど含まないカーボンナノチューブ単独の構造体として形成されることを特徴としており、本発明の生体適合性材料は上記集合体からなることを特徴とする。生体的合成材料としては、人工関節材料、歯科用材料、人工骨材料が好ましい。本発明の電気電子材料は上記集合体からなることを特徴とする。電気電子材料としては、生体電極材料、電池電極材料、燃料電池電極材料、電気二重層キャパシタ電極材料が好ましい。
また、本発明ではカーボンナノチューブをフッ素(F2)ガスと反応させることにより、フッ素化する。フッ素ガス濃度は特に限定されるものではないが、0.1〜100%、好ましくは1〜80%、より好ましくは1〜50%のものがフッ素ガスの取扱いから好ましい。フッ素ガスの希釈には例えば不活性ガス(He、Ar、N2)を用いると良い。
金属汚染の確認はX線光電子分光装置を用い行なった。
集合体の作成(8)。未精製多層カーボンナノチューブを200℃、12時間の間、真空乾燥する。このサンプル(1g)を内径Φ20mm、高さ60mmのグラファイト製焼結ダイの中に充填する。焼結ダイをSPS装置に設置し、80MPaで圧縮した後、チャンバー内の脱気を行う。25℃/minで1000℃まで昇温して10min恒温処理した。放冷後、多層カーボンナノチューブ集合体は得られなかった。
集合体の作成(9)。実施例1で得られる精製多層カーボンナノチューブを200℃、12時間の間、真空乾燥する。このサンプル(1g)を内径Φ20mm、高さ60mmのグラファイト製焼結ダイの中に充填する。焼結ダイをSPS装置に設置し、80MPaで圧縮した後、チャンバー内の脱気を行う。25℃/minで1000℃まで昇温して10min恒温処理した。放冷後、多層カーボンナノチューブ集合体は得られなかった。
集合体の作成(10)。実施例9の処理で得られる欠陥導入多層カーボンナノチューブを200℃、12時間の間、真空乾燥する。このサンプル(1g)を内径Φ20mm、高さ60mmのグラファイト製焼結ダイの中に充填する。焼結ダイをSPS装置に設置し、80MPaで圧縮した後、チャンバー内の脱気を行う。25℃/minで1000℃まで昇温して10min恒温処理した。放冷後、多層カーボンナノチューブ集合体を得た。得られた集合体を加工することができた。
レゾール型フェノール樹脂(1g)をエチルアルコールに溶解し、そこへ実施例1で得られる精製多層カーボンナノチューブ(1g)を添加する。これに超音波を照射し、十分に撹拌してからエチルアルコールを蒸発させて、フェノール樹脂皮膜カーボンナノチューブを得た。これを窒素中200℃に加熱、2時間恒温することでフェノール樹脂を分解し、非晶性炭素添加カーボンナノチューブ原料とした。このサンプル(1.3g)を内径Φ20mm、高さ60mmのグラファイト製焼結ダイの中に充填する。焼結ダイをSPS装置に設置し、80MPaで圧縮した後、チャンバー内の脱気を行う。25℃/minで1000℃まで昇温して10min恒温処理した。放冷後、樹脂添加多層カーボンナノチューブ集合体を得た。得られた集合体を加工することができた。
実施例5乃至7、実施例10及び11と比較例3及び4で得られた多層カーボンナノチューブ集合体(焼結体)から、縦1mm×横20mm×高さ1mmの試験片を作成する。得られた試験片の表面を#1200の研磨紙により平滑にし、次に#2000のラッピングテープにより先の研磨で生じた研磨痕を除去した。さらに#4000のラッピングテープにより仕上げを行った。研磨後のサンプル表面を光学顕微鏡により観察し、微小な傷がない試験片に対して、3点曲げ試験を行い機械的強度(曲げ強度、ヤング率)の測定を行った。尚、3つのサンプルを用意し、それらの平均値を求めた。
実施例6および比較例4で得られた多層カーボンナノチューブ集合体(焼結体)から縦1mm×横5mm×高さ1mmの試験片を作成する。得られた試験片の表面を#1200の研磨紙により平滑にし、次に#2000のラッピングテープにより先の研磨で生じた研磨痕を除去した。さらに#4000のラッピングテープにより仕上げを行った。全身麻酔下で、6週齢ウィスター系オスラットの腹部皮下に形成したポケット内に作成した試験片を埋入して、1週後に屠殺し、周囲組織とともに摘出し固定した。可及的丁寧にサンプルを除去後、通法に従いパラフィンに包埋して、薄切後ヘマトキシリン・エオジン染色を行い組織学的に検索し、親和性を判断した。図7に試験片周辺組織の観察写真を示す。
Claims (15)
- (1)カーボンナノチューブにフッ素修飾をする工程、(2)フッ素修飾した複数のカーボンナノチューブを焼結する工程からなることを特徴とするカーボンナノチューブ集合体の形成方法。
- 非酸化性雰囲気中で、形成温度が250〜3000℃であることを特徴とする請求項1記載のカーボンナノチューブ集合体の形成方法。
- 非酸化性雰囲気中で、形成圧力が10〜600MPaであることを特徴とする請求項1又は2記載のカーボンナノチューブ集合体の形成方法。
- 前記フッ素修飾をする工程を、フッ素系樹脂からなる容器内において、フッ素(F2)ガスで処理することを特徴とする請求項1乃至3のいずれか1項記載のカーボンナノチューブ集合体の形成方法。
- 前記フッ素系樹脂は、パーフルオロ化したフッ素系樹脂であることを特徴とする請求項4記載のカーボンナノチューブ集合体の形成方法。
- 前記カーボンナノチューブが単層ナノチューブであることを特徴とする請求項1乃至5のいずれか1項記載のカーボンナノチューブ集合体の形成方法。
- 前記カーボンナノチューブが多層ナノチューブであることを特徴とする請求項1乃至5のいずれか1項記載のカーボンナノチューブ集合体の形成方法。
- 前記カーボンナノチューブが欠陥導入されたカーボンナノチューブであることを特徴とする請求項1乃至7のいずれか1項記載のカーボンナノチューブ集合体の形成方法
- 複数のカーボンナノチューブ同士を結合させてなることを特徴とするカーボンナノチューブ集合体。
- 請求項1乃至8のいずれか1項記載の形成方法で形成したことを特徴とするカーボンナノチューブの集合体。
- 請求項1乃至8のいずれか1項記載の形成方法で形成したことを特徴とする請求項9記載のカーボンナノチューブ集合体
- 請求項9乃至11の集合体からなることを特徴とする生体適合性材料。
- 人工関節材料、歯科用材料、人工骨材料であることを特徴とする請求項12記載の生体適合性材料。
- 請求項9乃至11の集合体からなることを特徴とする電気電子材料。
- 生体電極材料、電池電極材料、燃料電池電極材料、電気二重層キャパシタ電極材料であることを特徴とする請求項14記載の電気電子材料。
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JP2005219950A (ja) * | 2004-02-04 | 2005-08-18 | Nikon Corp | 炭素材料、炭素材料の製造方法、ガス吸着装置及び複合材料 |
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AU6044599A (en) * | 1998-09-18 | 2000-04-10 | William Marsh Rice University | Chemical derivatization of single-wall carbon nanotubes to facilitate solvation thereof; and use of derivatized nanotubes |
JP4863590B2 (ja) | 2001-08-24 | 2012-01-25 | 双葉電子工業株式会社 | カーボンナノチューブの改質方法、カーボンナノチューブ及び電子放出源 |
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JPH0624720A (ja) * | 1992-07-06 | 1994-02-01 | Idemitsu Kosan Co Ltd | フッ素化フラーレンの製造方法 |
JP2002134325A (ja) * | 2000-07-08 | 2002-05-10 | Lg Electronics Inc | カーボンナノチューブ及び/またはカーボンナノファイバーを利用したインダクター |
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JP2006511434A (ja) * | 2002-11-27 | 2006-04-06 | ウィリアム・マーシュ・ライス・ユニバーシティ | 官能基化カーボンナノチューブポリマー複合体および放射線との相互作用 |
JP2004352608A (ja) * | 2003-05-28 | 2004-12-16 | Samsung Corning Co Ltd | 炭素ナノ構造体の分散方法 |
JP2005219950A (ja) * | 2004-02-04 | 2005-08-18 | Nikon Corp | 炭素材料、炭素材料の製造方法、ガス吸着装置及び複合材料 |
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US7740825B2 (en) | 2010-06-22 |
US20070209093A1 (en) | 2007-09-06 |
TWI359840B (ja) | 2012-03-11 |
JP5014786B2 (ja) | 2012-08-29 |
WO2005095274A1 (ja) | 2005-10-13 |
TW200535183A (en) | 2005-11-01 |
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