JP5334278B1 - 炭素繊維材、炭素繊維材製造方法、前記炭素繊維材を有する材 - Google Patents
炭素繊維材、炭素繊維材製造方法、前記炭素繊維材を有する材 Download PDFInfo
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- JP5334278B1 JP5334278B1 JP2013505242A JP2013505242A JP5334278B1 JP 5334278 B1 JP5334278 B1 JP 5334278B1 JP 2013505242 A JP2013505242 A JP 2013505242A JP 2013505242 A JP2013505242 A JP 2013505242A JP 5334278 B1 JP5334278 B1 JP 5334278B1
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Images
Classifications
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Abstract
本発明は、分散液作製工程と遠心紡糸工程と変性工程とを具備する炭素繊維材の製造方法であって、前記分散液作製工程は樹脂および炭素粒子を含む分散液が作製される工程であり、前記遠心紡糸工程は前記分散液から炭素繊維前駆体からなる不織布が作製される工程であり、前記変性工程は前記炭素繊維前駆体が炭素繊維に変性する工程である。
Description
分散液作製工程と遠心紡糸工程と変性工程とを具備する炭素繊維材の製造方法であって、
前記分散液作製工程は、樹脂および炭素粒子を含む分散液が作製される工程であり、
前記遠心紡糸工程は、前記分散液から、炭素繊維前駆体よりなる不織布が作製される工程であり、
前記変性工程は、前記炭素繊維前駆体が炭素繊維に変性する工程である
ことを特徴とする炭素繊維材製造方法によって解決される。
ことを特徴とする炭素繊維材によって解決される。
前記分散液は、樹脂および炭素粒子を含む。
前記樹脂は、好ましくは、溶媒(遠心紡糸時に揮発する溶媒)に溶解する樹脂である。具体的には、ビニル樹脂(例えば、ポリビニルアルコール(PVA)、ポリビニルブチラール(PVB)など)である。又は、ポリエチレンオキサイド(PEO)である。又は、アクリル樹脂(例えば、ポリアクリル酸(PAA)、ポリメチルメタアクリレート(PMMA)、ポリアクリロニトリル(PAN)など)である。又は、フッ素樹脂(例えば、ポリビニリデンジフルオリド(PVDF)など)である。又は、天然物由来高分子(例えば、セルロース樹脂およびその誘導体(ポリ乳酸、キトサン、カルボキシメチルセルロース(CMC)、ヒドロキシエチルセルロース(HEC)など)である。又は、ポリエーテルスルホン(PES)などのエンジニアリングプラスチック樹脂である。又は、ポリウレタン樹脂(PU)である。又は、ポリアミド樹脂(ナイロン)である。又は、芳香族ポリアミド樹脂(アラミド樹脂)である。又は、ポリエステル樹脂である。又は、ポリスチレン樹脂である。又は、ポリカーボネート樹脂である。又は、前記樹脂の混合物や共重合体である。
例えば、図1,2の遠心紡糸装置が用いられる。図1は遠心紡糸装置の概略側面図である。図2は遠心紡糸装置の概略平面図である。図中、1は、中が空洞で壁面にノズル又は穴の開いた回転体(円盤)である。前記円盤1の内部(空洞部)2(図示せず)に紡糸原液が充填される。円盤1が高速回転させられる。これによって、紡糸原液が遠心力によって引き伸ばされる。そして、溶媒は揮発しつつ、捕集板3上に堆積する。この堆積によって、不織布4が形成される。
[前記前駆体製不織布の熱処理(工程III−1)]
炭素繊維製の不織布が前記炭素繊維前駆体製の不織布から得られる。これは、前記炭素繊維前駆体が炭素繊維に変性されることで得られる。変性処理は、例えば熱処理である。特に、酸化性ガス雰囲気下での熱処理である。この熱処理により、前記炭素繊維前駆体を構成している樹脂が除去される。すなわち、炭素粒子以外の炭素源が除去される。かつ、前記炭素粒子の不融化が行われる。
炭素繊維製の不織布を得る為、好ましくは、炭化処理が行われる。この炭化処理は熱処理である。好ましくは、不活性ガス雰囲気下での熱処理である。本工程を経て、前記不融化炭素繊維前駆体が炭素繊維になる。本工程は、好ましくは、前記工程III−1の後に行われる。
好ましくは、黒鉛化処理が行われる。黒鉛化処理は、好ましくは、不活性ガス雰囲気下で行われる。本工程は、不織布がリチウムイオン電池の負極材などに用いられる場合、大事な工程である。本工程は、好ましくは、前記工程III−2の後に行われる。
本工程は、前記工程で得られた不織布から炭素繊維を得る工程である。本工程は、例えば前記工程II、前記工程III−1、若しくは前記工程III−2、又は前記工程III−3で得られた不織布が粉砕される工程である。好ましくは、前記工程III−2,III−3で得られた不織布が粉砕される工程である。前記粉砕によって繊維が得られる。前記不織布が叩かれることによっても、前記不織布は解かれ、繊維が得られる。
メディアレスミルが用いられると、繊維の潰れが防止される。従って、メディアレスミルの採用は好ましい。例えば、エアージェットミルや超音波照射の採用は好ましい。
粉砕後に繊維形状以外の材が含まれている場合は、好ましくは、分級工程が採用される。例えば、気流分級(サイクロン分級)や篩分級が採用されることが好ましい。
前記炭素繊維不織布(又は前記炭素繊維)は、電気素子(電子素子も電気素子の中に含まれる)の部材に用いられる。例えば、蓄電池、キャパシタ、燃料電池などの部材に用いられる。
前記炭素繊維不織布(又は前記炭素繊維)は、粒子の捕集あるいは分級に用いられる。すなわち、フィルタとして用いられる。
本発明の炭素繊維は高分子複合材の導電助剤として用いることが出来る。母材となる高分子には、格別な制限はない。例えば、ポリカーボネート、ポリメチルメタアクリレート、ABS樹脂、ホリオレフィン(ポリエチレン、ポリプロピレン)等の樹脂(硬質な樹脂)が挙げられる。又、軟質な樹脂であっても良い。例えば、ポリ塩化ビニル、天然ゴム、スチレンブタジエンゴムなどでも良い。アクリル系の粘着材であっても良い。光硬化性樹脂であっても良い。エポキシ樹脂、ポリビニルアルコールや澱粉などの接着剤であっても良い。添加量は、高分子材の種類によって異なる。炭素繊維の添加量(含有量)が多すぎると、成型が困難になる。逆に、少なすぎると、導電性が低下する。従って、炭素繊維の含有量は0.01〜80質量%が好ましい。より好ましくは0.1質量%以上である。30質量%以下である。
70質量部のポリビニルアルコール(商品名:ポバール117:株式会社クラレ製)と、30質量部のメソフェーズピッチ(商品名:AR:三菱ガス化学株式会社社製)と、400質量部の水とが、ビーズミルで、混合された。これにより、ポリビニルアルコールが溶解したメソフェーズピッチ分散液が作製された。
90質量部のポリビニルアルコール(商品名:ポバール117:株式会社クラレ製)と、10質量部のメソフェーズピッチ(商品名:AR:三菱ガス化学株式会社社製)と、900質量部の水とが、ビーズミルで、混合された。これにより、ポリビニルアルコールが溶解したメソフェーズピッチ分散液が作製された。
実施例1において、90質量部のポリビニルアルコール(商品名:ポバール117:株式会社クラレ製)と、10質量部のメソフェーズピッチ(商品名:AR:三菱ガス化学株式会社社製)と、400質量部の水とした以外は、同様に行われた。この結果、実施例1と同等な炭素繊維製不織布が得られた。
実施例1において、ポリビニルアルコールの代わりに、ポリアクリル酸(商品名:アクアリックAS58:株式会社日本触媒製)が用いられた以外は、同様に行われた。この結果、実施例1と同等な炭素繊維製不織布が得られた。
電極が作製された。この電極の負極活物質は実施例1の不織布である。
実施例1で得られた炭素繊維製の不織布10mgがガラス瓶に入れられた。更に、水が10g投入された。この後、超音波が照射された。超音波照射により前記炭素繊維が解かれた。すなわち、炭素繊維が得られた。得られた炭素繊維分散水がフィルタで濾過され、炭素繊維が回収された。
実施例5において、実施例1で得られた炭素繊維性不織布の代わりに比較例1で得られた炭素繊維性不織布が用いられた以外は同様に行われた。そして、リチウムイオン二次電池用正極が作製された。
実施例5で得られた0.5質量部の炭素繊維と、10質量部のポリビニルアルコール水溶液(固形分濃度15wt%)とが混合された。この混合物(複合材)がアルミニウム箔上に塗布(膜厚:1mm)された。塗膜の上にアルミニウム箔が積層された。このものが、60℃にて、12時間、乾燥処理された。そして、2枚のアルミニウム箔が前記複合材で接着された。
60質量部のポリビニルアルコール(商品名:ポバール224:株式会社クラレ製)と、40質量部のメソフェーズピッチ(商品名:AR:三菱ガス化学株式会社社製)と、900質量部の水とが、ビーズミルで、混合された。これにより、ポリビニルアルコールが溶解したメソフェーズピッチ分散液が作製された。
遠心紡糸装置(図1,2参照 ノズルと捕集体との距離;1.3m 円盤回転数:12,000rpm)が用いられた。すなわち、上記分散液(共軸二重円筒型粘度計(測定装置:BH型粘度計:TOKIMEC社製)による粘度:1000mPa・S)を用いて遠心紡糸が行われた。炭素繊維前駆体製の不織布が捕集板上に作製された。この方法によれば、1時間で、黒鉛化後の重量に換算して20kg相当の紡糸を行うことが出来た。
この後、アルゴンガス雰囲気下で、800℃までの加熱が行われた。
次いで、黒鉛化炉にて、3000℃までの加熱が行われた。
得られた不織布のSEM写真(SEM装置:VE−8800 株式会社KEYENCE製)が図9に示される。この不織布における炭素繊維は、炭素繊維の径が大きな大径部(直径が20nm〜5μm)と、炭素繊維の径が小さな小径部(10nm〜3μm)とを有するものであった。勿論、(前記大径部における直径)>(前記小径部における直径)である。
X線回折測定の結果が図10に示される。これによれば、黒鉛構造(002)由来のピークが25°〜30°(2θ)の範囲に有った。前記ピークの半値幅は0.1〜2であった。
BET法による比表面積は8.98m2/gであった。
得られた炭素繊維不織布がジェットミルにて粉砕された。この後、サイクロン分級が行われた。このようにして得られた炭素繊維のSEM写真が図11に示される。
この炭素繊維が用いられ、実施例5と同様に行われ、リチウムイオン二次電池用正極が作製された。
この正極の表面電気抵抗が、4端子法(三菱化学アナリテック社製)により、測定された。その結果は、0.1Ω/□であった。
対極にリチウムが用いられ、充・放電測定が行われた。この結果が図12に示される。
これによれば、本実施例の炭素繊維はリチウムイオン二次電池導電助材に好適であることが判る。
2 内部(空洞部)
3 捕集板
4 不織布
Claims (21)
- 分散液作製工程と遠心紡糸工程と変性工程とを具備する炭素繊維材の製造方法であって、
前記分散液作製工程は、樹脂および炭素粒子を含む分散液が作製される工程であり、
前記遠心紡糸工程は、前記分散液から、炭素繊維前駆体よりなる不織布が作製される工程であり、
前記変性工程は、前記炭素繊維前駆体が炭素繊維に変性する工程である
ことを特徴とする炭素繊維材製造方法。 - 遠心紡糸工程に供された分散液は、共軸二重円筒型粘度計による粘度が10〜10000mPa・Sである
ことを特徴とする請求項1の炭素繊維材製造方法。 - 遠心紡糸工程に供された分散液は、固形分濃度が0.1〜50質量%である
ことを特徴とする請求項1又は請求項2の炭素繊維材製造方法。 - 遠心紡糸工程における遠心紡糸装置の円盤の回転数が1000〜100000rpmである
ことを特徴とする請求項1〜請求項3いずれかの炭素繊維材製造方法。 - 遠心紡糸工程に供された分散液は少なくともピッチを含む
ことを特徴とする請求項1〜請求項4いずれかの炭素繊維材製造方法。 - 更に不織布が解かれる解布工程を具備してなり、
炭素繊維材が炭素繊維である
ことを特徴とする請求項1〜請求項5いずれかの炭素繊維材製造方法。 - 解布工程がメディアレスミル法による
ことを特徴とする請求項6の炭素繊維製造方法。 - 解布工程がエアージェットミル法による
ことを特徴とする請求項6の炭素繊維製造方法。 - 解布工程が超音波照射法による
ことを特徴とする請求項6の炭素繊維製造方法。 - 解布工程の後に分級工程を具備する
ことを特徴とする請求項6〜請求項9いずれかの炭素繊維材製造方法。 - 請求項1〜請求項10いずれかの炭素繊維製材製造方法によって得られてなる
ことを特徴とする炭素繊維材。 - 炭素繊維材の炭素繊維は、炭素繊維の径が大きな大径部と、炭素繊維の径が小さな小径部とを有し、
前記大径部は、その直径が20nm〜5μmであり、
前記小径部は、その直径が10nm〜3μmであり、
(前記大径部における直径)>(前記小径部における直径)である
ことを特徴とする請求項11の炭素繊維材。 - 電気デバイスに用いられる部材であって、
前記部材は、請求項11または請求項12の炭素繊維材を用いて構成されてなる
ことを特徴とする電気デバイスに用いられる部材。 - 部材が電池の電極である
ことを特徴とする請求項13の電気デバイスに用いられる部材。 - 部材がリチウムイオン二次電池の電極である
ことを特徴とする請求項13の電気デバイスに用いられる部材。 - 部材がリチウムイオン二次電池の電極であり、炭素繊維材からなる導電助剤を含む
ことを特徴とする請求項13の電気デバイスに用いられる部材。 - 部材がキャパシタの電極である
ことを特徴とする請求項13の電気デバイスに用いられる部材。 - 部材が燃料電池用多孔質炭素電極基材である
ことを特徴とする請求項13の電気デバイスに用いられる部材。 - 電気デバイスであって、
請求項13〜請求項18いずれかの電気デバイスに用いられる部材を具備してなることを特徴とする電気デバイス。 - フィルタであって、
前記フィルタは、請求項11または請求項12の炭素繊維材を用いて構成されてなる
ことを特徴とするフィルタ。 - 高分子複合材であって、
前記高分子複合材は、請求項11または請求項12の炭素繊維材を用いて構成されてなる
ことを特徴とする高分子複合材。
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