JP5744008B2 - 複合材料構造体を除氷するためのcntベース抵抗加熱 - Google Patents
複合材料構造体を除氷するためのcntベース抵抗加熱 Download PDFInfo
- Publication number
- JP5744008B2 JP5744008B2 JP2012508572A JP2012508572A JP5744008B2 JP 5744008 B2 JP5744008 B2 JP 5744008B2 JP 2012508572 A JP2012508572 A JP 2012508572A JP 2012508572 A JP2012508572 A JP 2012508572A JP 5744008 B2 JP5744008 B2 JP 5744008B2
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- JP
- Japan
- Prior art keywords
- cnt
- carbon
- fiber material
- cnts
- carbon fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B64—AIRCRAFT; AVIATION; COSMONAUTICS
- B64D—EQUIPMENT FOR FITTING IN OR TO AIRCRAFT; FLIGHT SUITS; PARACHUTES; ARRANGEMENTS OR MOUNTING OF POWER PLANTS OR PROPULSION TRANSMISSIONS IN AIRCRAFT
- B64D15/00—De-icing or preventing icing on exterior surfaces of aircraft
- B64D15/12—De-icing or preventing icing on exterior surfaces of aircraft by electric heating
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C04B2235/5208—Fibers
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/5208—Fibers
- C04B2235/5264—Fibers characterised by the diameter of the fibers
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5284—Hollow fibers, e.g. nanotubes
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- H—ELECTRICITY
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- H05B2214/00—Aspects relating to resistive heating, induction heating and heating using microwaves, covered by groups H05B3/00, H05B6/00
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Description
本願は、2009年4月27日出願の米国仮特許出願第61/173,027号に基づいて優先権を主張するものであり、参照により全体が本明細書に組み込まれる。
当該技術分野で知られている標準的なCNT合成反応器は横断面が円形である。これには、例えば、歴史的理由(研究所では円筒状の反応器がよく用いられる)及び利便性(流体力学は円筒状の反応器にモデル化すると容易であり、また、加熱器システムは円管チューブ(石英など)に容易に対応する)、並びに製造の容易性などの多くの理由がある。本願発明は、従来の円筒形状と一線を画して、矩形横断面を有するCNT合成反応器を提供する。脱却した理由は以下の通りである。1.反応器により処理される多数の炭素繊維材料は、例えば、形状が薄いテープやシート状など相対的に平面的であるので、円形横断面では反応器の容積を効率的に使用していない。この非効率性は、円筒状のCNT合成反応器にとって、例えば、以下のa)ないしc)に挙げるような、いくつかの欠点となる。a)十分なシステムパージの維持;反応器の容積が増大すれば、同レベルのガスパージを維持するためにガス流量の増大が必要になる。これは、開放環境におけるCNTsの大量生産には非効率なシステムとなる。b)炭素原料ガス流量の増大;前記a)のように、不活性ガス流を相対的に増大させると、炭素原料ガス流量を増大させる必要がある。12Kの炭素繊維トウは、矩形横断面を有する合成反応器の全容積に対して2000分の1の容積であることを考慮されたい。同等の円筒状の成長反応器(すなわち、矩形横断面の反応器と同じ平坦化された炭素繊維材料を収容できるだけの幅を有する円筒状の反応器)では、炭素繊維材料は、チャンバー容積の17,500分の1の容積である。CVDなどのガス蒸着処理(gas deposition processes)は、通常、圧力及び温度だけで制御されるが、容積は蒸着の効率に顕著な影響を与える。矩形反応器の場合、それでもなお過剰な容積が存在する。この過剰容積は無用の反応を促進してしまうが、円筒状反応器は、その容積が約8倍もある。このように競合する反応が発生する機会が増加することにより、所望の反応が有効に生じるには、円筒状反応器チャンバーでは遅くなってしまう。このようなCNT成長の減速は連続処理の進行には問題となる。矩形反応器の構成の利点の1つは、矩形チャンバーの高さを低くすることで反応器の容積が低減され、これにより容積比が改善され反応がより効率的になるという点である。本願発明のある実施形態において、矩形合成反応器の全容積は、合成反応器を通過中の炭素繊維材料の全容積に対して僅か約3000倍にしかすぎない。またある実施形態では、矩形合成反応器の全容積は、合成反応器を通過中の炭素繊維材料の全容積に対して僅か約4000倍にしかすぎない。また更なる実施形態では、矩形合成反応器の全容積は、合成反応器を通過中の炭素繊維材料の全容積に対して約10,000倍以下である。加えて、円筒状反応器を使用した場合、矩形横断面を有する反応器と比較すると、同じ流量比を供給するためには、より大量の炭素原料が必要である点に注目されたい。当然のことながら、実施形態の中には、合成反応器が、矩形ではないが比較的矩形に類似する多角形状で表される横断面を有し、円形横断面を有する反応器に対して反応器の容積を同様に低減するものがある。c)問題のある温度分布;相対的に小径の反応器が用いられた場合、チャンバー中心からその壁面までの温度勾配はごく僅かである。しかし、例えば、工業規模の生産に用いられるなど、サイズの増大に伴い、温度勾配は増加する。このような温度勾配により、炭素繊維材料基材の全域で製品品質がばらつく結果となる(すなわち、製品品質が半径位置の関数として変化する)。この問題は、矩形横断面を有する反応器を用いた場合に殆ど回避される。特に、平面的な基材が用いられる場合、基材のサイズが大きくなったときに、反応器の高さを一定に維持することができる。反応器の頂部と底部間の温度勾配は基本的にごく僅かであり、結果的に、生じる熱的な問題や製品品質のばらつきは回避される。2.ガス導入:当該技術分野では、通常、管状炉が使用されているので、一般的なCNT合成反応器は、ガスを一端に導入し、それを反応器に通して他端から引き出している。本明細書に開示された実施形態の中には、ガスが、反応器の両側面又は反応器の頂面及び底面のいずれかを通して対称的に、反応器の中心又は対象とする成長ゾーン内に導入されるものがある。これにより、流入する原料ガスがシステムの最も高温の部分(CNT成長が最も活発な場所)に連続的に補充されるので、全体的なCNT成長速度が向上する。このような一定のガス補充は、矩形のCNT反応器により示される成長速度の向上にとって重要な側面である。
比較的低温のパージゾーンを提供するチャンバーが矩形合成反応器の両端に従属する。出願人は、仮に高温ガスが外部環境(すなわち、反応器の外部)と接触したならば、炭素繊維材料の分解が増加するだろうと判断した。低温パージゾーンは、内部システムと外部環境間の緩衝となる。当該技術分野で知られている標準的なCNT合成反応器の構成では、通常、基材を慎重に(かつ緩やかに)冷却することが求められる。本願の矩形CNT成長反応器の出口における低温パージゾーンは、連続的なインライン処理に必要とされるような短時間の冷却を実現する。
ある実施形態において、金属製、特にステンレス鋼のホットウォール型(hot-walled)反応器が使用される。このことは、金属、特にステンレス鋼は炭素を析出(すなわち、すす及び副生成物の形成)しやすいため、常識に反するようにも考えられる。このように、大部分のCNT反応器の構造には、炭素の析出が少なく、また、石英は洗浄しやすく、試料の観察が容易であることから、石英反応器が使用されている。しかしながら、出願人は、ステンレス鋼上にすす及び炭素析出物が増加することにより、より着実、高速、効率的かつ安定的なCNT成長がもたらされるという点に着眼した。理論に拘束されるものではないが、大気圧運転(atmospheric operation)と連動して、反応器内で生じるCVD処理では拡散が制限されることが示されている。すなわち、触媒に「過度に供給される(overfed)」、つまり、過量の炭素が(反応器が不完全真空下で運転している場合よりも)その相対的に高い分圧により反応器システム内で得られる。結果として、開放システム(特に清浄なもの)では、過量の炭素が触媒粒子に付着してCNTsの合成能力を低下させる。ある実施形態において、金属反応器壁にすすが析出して反応器に「汚れが付いて(dirty)」いる場合に、矩形反応器を意図的に運転する。炭素が反応器壁上の単分子層に一度析出すると、炭素は、それ自体を覆って析出しやすくなる。得られる炭素の中には、この機構により「回収される(withdrawn)」ものがあるので、ラジカルの形で残っている炭素原料が、触媒を被毒させない速度で触媒と反応する。既存のシステムが「清浄に」運転しても、連続処理のために開放状態であれば、成長速度が低下してCNTsの生産量は著しく低下する。
本明細書に開示されたCNT合成反応器において、触媒還元及びCNT成長のいずれもが反応器内で生じる。還元工程は、個別の工程として実施されると、連続処理に用いるものとして十分タイムリーには行われなくなるため、このことは重要である。当該技術分野において知られている標準的な処理において、還元工程の実施には、通常1〜12時間かかる。本願発明によれば、両工程は1つの反応器内で生じるが、これは、少なくとも1つには、炭素原料ガスを導入するのが、円筒状反応器を用いる当該技術分野では標準的となっている反応器の端部ではなく、中心部であることによる。還元処理は、繊維が加熱ゾーンに入ったときに行われる;この時点に至るまでに、ガスには、触媒と反応して(水素ラジカルの相互作用により)酸化還元を引き起こす前に反応器壁と反応して冷える時間があるということである。還元が起こるのは、この移行領域である。システム内で最も高温の等温ゾーンでCNTの成長は起こり、反応器の中心近傍におけるガス入口の近位で最速の成長速度が生じる。
Claims (27)
- 航空機の構造部材用に適合され航空機の飛行により生じる荷重を支える機体と、
前記機体の一部に内包される繊維基材と、
前記繊維基材に対して垂直に配列かつ配向されるように前記繊維基材上にその場で成長し、これにより、カーボン・ナノチューブ浸出繊維材料を形成する、複数のカーボン・ナノチューブと、
前記カーボン・ナノチューブ浸出繊維材料を含む前記機体の前記一部と電気的に接続され、前記カーボン・ナノチューブ浸出繊維材料に電流を流して、前記カーボン・ナノチューブ浸出繊維材料の内部に熱を生じさせ、これにより前記機体を加熱して、除氷し、あるいは、前記機体の表面における氷形成を抑制する、第1の電極及び第2の電極と、
を含んで構成された複合材料構造体。 - 前記機体が、航空機の主翼の一部を形成するように適合された、請求項1に記載の複合材料構造体。
- 前記機体が、ヘリコプターのブレードの一部を形成するように適合された、請求項1に記載の複合材料構造体。
- 前記機体が、航空機の推進器翼の一部を形成するように適合された、請求項1に記載の複合材料構造体。
- 前記繊維基材がガラスを含んで構成された請求項1に記載の複合材料構造体。
- 前記繊維基材が炭素を含んで構成された請求項1に記載の複合材料構造体。
- 前記繊維基材がセラミックを含んで構成された請求項1に記載の複合材料構造体。
- 前記複数のカーボン・ナノチューブが、単層カーボン・ナノチューブ、2層カーボン・ナノチューブ、多層カーボン・ナノチューブ、及びこれらを混合したものからなる群より選択されるカーボン・ナノチューブとして成長した、請求項1に記載の複合材料構造体。
- 前記複数のカーボン・ナノチューブは、通常、長さが均一となり、かつ、分布が均一となるまで成長した、請求項1に記載の複合材料構造体。
- 前記複数のカーボン・ナノチューブが、1ミクロンから500ミクロンの長さを有するまで成長した、請求項1に記載の複合材料構造体。
- 前記複数のカーボン・ナノチューブが、1ミクロンから10ミクロンの長さを有するまで成長した、請求項1に記載の複合材料構造体。
- 前記複数のカーボン・ナノチューブが、10ミクロンから100ミクロンの長さを有するまで成長した、請求項1に記載の複合材料構造体。
- 前記複数のカーボン・ナノチューブが、100ミクロンから500ミクロンの長さを有するまで成長した、請求項1に記載の複合材料構造体。
- 前記複数のカーボン・ナノチューブが、1μm 2 当たり最大15,000のナノチューブの密度を特徴とする分布の均一性を有するまで成長した、請求項1に記載の複合材料構造体。
- 前記繊維基材は、フィラメント、トウ、ヤーン、テープ、一方向テープ、繊維ブレイド、織物、不織繊維マット、繊維プライ、及び3次元織物構造体から選択される請求項1に記載の複合材料構造体。
- 前記カーボン・ナノチューブ浸出繊維材料が、前記機体の表面付近に配置された請求項1に記載の複合材料構造体。
- 前記カーボン・ナノチューブ浸出繊維材料が、前記機体の全体にわたって配置された請求項1に記載の複合材料構造体。
- 前記電流が、1ボルトから24ボルトの直流電圧の印加により生じる、請求項1に記載の複合材料構造体。
- 前記電流が、60ボルトから480ボルトの交流電圧の印加により生じる、請求項1に記載の複合材料構造体。
- 前記カーボン・ナノチューブ浸出繊維材料を有する前記機体の前記一部に分散したマトリックス材を更に含んで構成された請求項1に記載の複合材料構造体。
- 前記マトリックス材が、エポキシ、フェノール樹脂、セメント、ガラス、熱可塑性物質及び熱硬化性物質からなる群の1以上の物質を含んで構成された、請求項20に記載の複合材料構造体。
- 前記マトリックス材の中に配置された複数の遊離したカーボン・ナノチューブを更に含んで構成された請求項20に記載の複合材料構造体。
- 航空機の飛行によって生じる荷重を支える航空機の構造部材のマトリックス内に組み込まれることにより複合材料を形成する複数のカーボン・ナノチューブ浸出繊維を含んで構成され、
前記カーボン・ナノチューブ浸出繊維は、繊維基材に対して垂直に配列かつ配向されるように前記繊維基材上にその場で成長した複数のカーボン・ナノチューブを含んで構成され、
前記複合材料が、電流を受けるように適合され、前記電流に反応して抵抗加熱素子として作用する除氷用製品。 - 前記マトリックスがカーボン・ナノチューブでドープされた請求項23に記載の除氷用製品。
- カーボン・ナノチューブが繊維基材に対して垂直に配列かつ配向されるように、前記繊維基材上にその場で複数のカーボン・ナノチューブを成長させて、これにより、カーボン・ナノチューブ浸出繊維材料を形成すること、
前記カーボン・ナノチューブ浸出繊維材料を一部に内包する機体を備え、かつ、航空機の飛行により生じる荷重を支えるように適合された、航空機の複合材料構造体を形成すること、及び
前記カーボン・ナノチューブ浸出繊維材料を含んで構成される前記機体の前記一部に第1の電極及び第2の電極を電気的に接続して、第1の電極及び第2の電極並びにその間の前記カーボン・ナノチューブ浸出繊維に電流を流すことで、前記カーボン・ナノチューブ浸出繊維材料の内部に熱を生じさせ、これにより前記複合材料構造体の前記機体を加熱して、除氷し、あるいは、前記複合材料構造体の表面における氷形成を抑制すること、
を含んで構成された方法。 - 前記電流の印加には、1ボルトから24ボルトの直流電圧を印加することが含まれる請求項25に記載の方法。
- 前記電流の印加には、60ボルトから480ボルトの直流電圧を印加することが含まれる請求項25に記載の方法。
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US17302709P | 2009-04-27 | 2009-04-27 | |
US61/173,027 | 2009-04-27 | ||
PCT/US2010/032446 WO2010129234A2 (en) | 2009-04-27 | 2010-04-26 | Cnt-based resistive heating for deicing composite structures |
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CN (1) | CN102460447A (ja) |
AU (1) | AU2010245098B2 (ja) |
BR (1) | BRPI1014711A2 (ja) |
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-
2010
- 2010-04-26 KR KR1020117025937A patent/KR101696207B1/ko active IP Right Grant
- 2010-04-26 JP JP2012508572A patent/JP5744008B2/ja not_active Expired - Fee Related
- 2010-04-26 EP EP10772494A patent/EP2425364A4/en not_active Withdrawn
- 2010-04-26 CN CN2010800290466A patent/CN102460447A/zh active Pending
- 2010-04-26 BR BRPI1014711A patent/BRPI1014711A2/pt not_active IP Right Cessation
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EP2425364A4 (en) | 2012-10-31 |
US20110024409A1 (en) | 2011-02-03 |
AU2010245098A1 (en) | 2011-11-03 |
ZA201108860B (en) | 2012-08-29 |
CN102460447A (zh) | 2012-05-16 |
WO2010129234A3 (en) | 2011-03-10 |
WO2010129234A2 (en) | 2010-11-11 |
KR101696207B1 (ko) | 2017-01-13 |
KR20120016622A (ko) | 2012-02-24 |
CA2760144A1 (en) | 2010-11-11 |
JP2012525476A (ja) | 2012-10-22 |
AU2010245098B2 (en) | 2014-11-13 |
US8664573B2 (en) | 2014-03-04 |
BRPI1014711A2 (pt) | 2016-04-12 |
EP2425364A2 (en) | 2012-03-07 |
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