JP5570686B2 - 微細炭素繊維分散皮膜およびその製造方法 - Google Patents
微細炭素繊維分散皮膜およびその製造方法 Download PDFInfo
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- JP5570686B2 JP5570686B2 JP2007122829A JP2007122829A JP5570686B2 JP 5570686 B2 JP5570686 B2 JP 5570686B2 JP 2007122829 A JP2007122829 A JP 2007122829A JP 2007122829 A JP2007122829 A JP 2007122829A JP 5570686 B2 JP5570686 B2 JP 5570686B2
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
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- BETUMLXGYDBOLV-UHFFFAOYSA-N tetradecyl 2-(trimethylazaniumyl)ethyl phosphate Chemical compound CCCCCCCCCCCCCCOP([O-])(=O)OCC[N+](C)(C)C BETUMLXGYDBOLV-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
- H10K85/221—Carbon nanotubes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Mathematical Physics (AREA)
- Theoretical Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
- Paper (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Description
カーボンナノ構造体を構成するグラファイト層は、通常では規則正しい六員環配列構造を有し、その特異な電気的性質とともに、化学的、機械的および熱的に安定した性質を持つ物質である。従って、皮膜形成成分中に、このような微細炭素繊維を均一かつ安定に分散配合することにより、前記したような物性を生かすことができれば、有望な導電性ないし制電性材料となり得る。また、このような微細炭素繊維分散皮膜は、上記に例示したような産業分野に限られず多方面での応用用途が期待されるものである。
本発明の炭素分散皮膜を得るにおいて、用いられる基板としては、炭素繊維分散液をその表面に展開できるものである限り特に限定されるものではなく、得ようとする炭素分散皮膜の用途等に応じて、各種の材質および各種の形状のものとすることができる。その材質としては、例えば、各種樹脂、各種ゴムないしエラストマー、ガラス、各種金属、各種セラミック、その他、紙、織布、編布、不織布、紐ないし糸等の各種繊維製品等のいずれのものを用いることができる。また、本発明の炭素分散皮膜は、このような基板上にそのまま残すことも、またこのような基板上から剥離して膜単体として得ることも可能であり、基板上にそのまま残す態様においては、対象となる基板は、例えば、所期の形状を有する製品ないし部品等であっても良い。一方、基板が最終製品としての皮膜単体から切り離される態様においては、基板は、このような皮膜に対しある程度、剥離性の良いものであることが望まれ、例えば、剥離紙や、表面に離型剤処理等を施した基板等を用いることができる。
次に、このような基板表面に膜状に展開される炭素繊維分散液としては、少なくとも炭素繊維およびこれを分散させる溶媒ないし分散媒を含むものである。
炭素繊維分散液中に配され、基板上に展開される微細炭素繊維としては、特に限定されるものではないが、主として、炭素の六員環配列構造を有する構造体であって、この構造体の三次元のディメンションのうち少なくとも1つの寸法がナノメートルの領域にある、たとえば、数〜数100nm程度のオーダーを有する、ものが代表的なものである。
炭素繊維分散液を調製する上で用いられる溶媒ないし分散媒としては、水系のものであっても、非水系のものであっても良く、炭素繊維分散液を展開する基材に対する安定性、濡れ性等の観点から適宜選択可能である。
本発明において用いられる炭素繊維分散液としては、上記したような溶媒ないし分散媒中に炭素繊維が均一に、より望ましくは、単分散状に安定に分散し得るものであれば、その分散方法としては、特に限定されるものではなく、従来、公知の各種の方法を単独であるいは複数組み合わせて、採択することは可能である。例えば、超音波処理、各種撹拌装置を用いた攪拌処理、加熱処理といった物理的方法、あるいは各種分散剤を分散液中に配合して分散液を調製する方法などを用いることができるが、好ましくは、分散剤を用いた分散方法である。
分散剤としては、使用する溶媒ないし分散媒の種類に応じて各種のものを用いることができる。
ここで、「リン脂質系界面活性剤」とは、リン酸基を官能基とする陰イオン性界面活性剤・両性イオン界面活性剤であり、リン脂質(グリセロリン脂質、スフィンゴリン脂質の両方を含む)及び改質リン脂質(例えば、水素添加リン脂質、リゾリン脂質、酵素変換リン脂質、リゾホスファチジルグリセロール、他の物質との複合体)のいずれでもよい。このようなリン脂質は、生物を構成する細胞の種々の膜系、例えば原形質膜、核膜、小胞体膜、ミトコンドリア膜、ゴルジ体膜、リソソーム膜、葉緑体膜、細菌細胞膜に存在し、好適には、リポソームの調製に用いられるリン脂質が好適である。具体的には、例えば、ホスファチジルコリン{例えば、ジステアロイルホスファチジルコリン(DSPC)、ジミリストイルホスファチジルコリン(DMPC)、ジパルミトリルホスファチジルコリン(DPPC)}、その他のレシチン、ホスファチジルエタノールアミン、ホスファチジルイノシトール、ホスファチジルセリン、ホスファチジルグリセロール、ジホスファチジルグリセロール、リゾホスファチジルコリン、スフィンゴミエリン、n−オクチルホスホコリン、n−ドデシルホスホコリン、n−テトラデシルホスホコリン、n−ヘキサデシルホスホコリンを挙げることができる。
炭素繊維の分散液中には、必要に応じてその他の成分を配合することが可能である。
上記したような炭素繊維分散液の基板上への膜状展開方法としては、特に限定されるものではなく、例えば、スピンコーティング法、スプレー法、ローラ法等のコーティング法、あるいは基板を炭素繊維分散液に浸漬する浸漬法などといった公知の各種方法を用いて、炭素繊維分散液を基板へ直接展開することによって行うことができる。
上記のように炭素繊維分散液の膜状展開層が少なくとも流動性を失った後に、当該膜状展開層に対して、前記皮膜基質を形成する皮膜形成成分を含有する流動体を適用する。
上記したように、炭素繊維分散液の膜状展開層が少なくとも流動性を失った後に、当該膜状展開層に対して、前記皮膜基質を形成する皮膜形成成分を含有する流動体を適用することによって、本発明の炭素繊維分散皮膜は基板上に形成されるが、このようにして形成された炭素繊維分散皮膜は、基板上より剥離してフィルム単体として得ることも、あるいは基板上にそのまま残した状態として得ることも可能である。
生成炉からの排ガスの一部を循環ガスとして使用し、この循環ガス中に含まれるメタン等の炭素化合物を、新鮮なトルエンと共に、炭素源として使用して、CVD法により微細炭素繊維を合成した。
精製水1リットルに対し、1.9グラムの3−(N,N−ジメチルステアリルアンモニオ)−プロパンスルホネート[3-(N,N-dimethylstearylammonio)-propanesulfonate]、0.1グラムのドデシル硫酸塩(dodecylsulfate)を添加し、混合ミセル水溶液を調製した。
ガラス基材の表面上に、合成例1で調製された微細炭素繊維の分散液を、所定の塗布量(乾燥重量換算:10mg/m2)でスピンコートによりコーティングし、80℃で2分間風乾させた。コーティングされた展開皮膜表面が乾燥した状態で、この上部より樹脂溶液(フェノール樹脂、濃度5%、溶剤:メタノール)を同様にスピンコートにより所定の塗布量(乾燥重量換算: 400mg/m2)でコーティングし、380℃で10分間熱乾させ、微細炭素繊維分散皮膜を形成した。この皮膜の表面抵抗率を測定したところ18Ω/□であった。また、耐スクラッチ性についても十分良好な特性を示した。
実施例1において、微細炭素繊維の分散液をコーティングし乾燥した後、再度微細炭素繊維の分散液をコーティングし乾燥するという工程を10回繰り返す以外は、実施例1と同様にして微細炭素繊維分散皮膜を形成した。得られた皮膜は、実施例1におけるものと同様に、表面抵抗率、耐スクラッチ性共に良好なものであった。
合成例1で調製された微細炭素繊維の分散液を、水槽に入れた精製水の界面に静かに滴下したところ、分散液は界面上に薄膜状に広がった。そして、基板をこの水面を通過して約10回上下させることで、基板表面に分散液の展開皮膜を転写し約20層に重畳させた。
Claims (3)
- 炭素繊維が皮膜基質中に分散されてなる炭素繊維分散皮膜であって、
前記炭素繊維が、筒状のグラフェンシートが軸直角方向に積層した構造であって、筒を構成するシートが多角形の軸直交断面を有し、該断面の最大径が15〜100nmであり、アスペクト比が105以下で、ラマン分光分析で514nmにて測定されるID/IGが0.1以下であり、
前記炭素繊維を、(a)水溶液中で直径が50〜2000nmの球状ミセルを形成し得る界面活性剤又は重量平均分子量が1万〜5千万である水溶性高分子よりなる分散剤、(b)微細炭素繊維透過性物質および(c)酸化剤を配合してなり、pHをアルカリ性とした分散媒ないし溶媒中に分散させ、
得られた分散媒ないし溶媒中に炭素繊維を分散させてなる炭素繊維分散液を、基板上に膜状に展開する工程および前記炭素繊維分散液の膜状展開層の少なくとも流動性を失わせる膜状展開層の非流動化の工程を、複数回繰り返した後、
当該膜状展開層に対して、前記皮膜基質を形成する皮膜形成成分を含有する流動体を適用し、皮膜形成成分を含有する溶液の塗布および乾燥、皮膜形成成分の溶融塗布および凝固、あるいは未架橋ないし未硬化の皮膜形成成分の塗布および架橋ないし硬化により前記皮膜基質を形成し、前記基板より剥離すること
で得られることを特徴とする炭素繊維分散皮膜。 - 前記炭素繊維として、外径15〜100nmの炭素繊維から構成される炭素繊維構造体であって、前記炭素繊維構造体は、前記炭素繊維が複数延出する態様で、当該炭素繊維を互いに結合する粒状部を有しており、かつ当該粒状部は前記炭素繊維の成長過程において形成されてなるものであることを特徴とする炭素構造体を含有するものである請求項1に記載の炭素繊維分散皮膜。
- 10-3〜108Ω/□の範囲内の表面抵抗率を有するものである請求項1または2に記載の炭素繊維分散皮膜。
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