JP5256307B2 - 黒鉛化フィルムを含む防火障壁保護材 - Google Patents
黒鉛化フィルムを含む防火障壁保護材 Download PDFInfo
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- JP5256307B2 JP5256307B2 JP2010550694A JP2010550694A JP5256307B2 JP 5256307 B2 JP5256307 B2 JP 5256307B2 JP 2010550694 A JP2010550694 A JP 2010550694A JP 2010550694 A JP2010550694 A JP 2010550694A JP 5256307 B2 JP5256307 B2 JP 5256307B2
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- B32B2307/212—Electromagnetic interference shielding
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- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/302—Conductive
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
- B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
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- B32B2307/5825—Tear resistant
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Description
フィルムにするためにキャスティング面にキャスティングされる。次に、一般的に、例えば、約80〜100℃にて加熱される。その結果、化学的な転化剤および触媒が活性化され、かつキャストフィルムがポリアミド酸/ポリイミドゲルフィルム(以下、「ゲルフィルム」という。)に転化される。加熱時間は、厚みによって決定される。約30秒〜10分加熱されることが好ましい。その後、このようにして得られたゲルフィルムは、水分、残った溶媒および化学的な転化剤を取り除くために加熱され、同時にポリアミド酸をポリイミドに転化する。
(A−B)×100/B
ここで、Aはゲルフィルムの重量を表し、Bは450℃で20分間加熱後のゲルフィルムの重量を表している。
(C/D)×100/(E/F)
ここで、Cは1370cm−1でのゲルフィルムの吸収ピークの高さを表し、Dは1500cm−1でのゲルフィルムの吸収ピークの高さを表し、Eは1370cm−1でのポリイミドフィルムの吸収ピークの高さを表し、Fは1500cm−1でのゲルフィルムの吸収ピークの高さを表している。
1.薄いこと
2.柔軟性を有すること
3.軽量であること
4.優れたバーンスルー(burn-through)耐性を有すること
5.水を吸収しないこと
6.ガスを発生させないこと
7.腐食されないこと。
シートの形成において与えられる防火障壁特性の程度を決定するために、試験体を評価した。黒鉛化ポリイミドシート(1milおよび1.5mil)、および3M社(3M Company)から入手したNEXTEL 312 フレームストッピングドットペーパー(Flame Stopping Dot Paper)のシートを、炎(flame challenge)に対する反応を決定するために評価した。黒鉛化ポリイミドシートを、4,4'−ジアミノジフェニルエーテルおよびピロメリト酸二無水物から得たポリイミドフィルムから作製した。
同一の試験を40μmの厚みを有する黒鉛化ポリイミドシートと、240μmの厚みを有する天然の黒鉛のシートとに対して行い、これらを比較した。両方の黒鉛シートに関する観察結果は、試験が完了した後に、天然の黒鉛のフィルムが、このシートの表面上に直径約2〜5mmの火ぶくれを形成したことに気づいたことを除いて、上述の観察結果と同一であった。しかし、炎は、天然の黒鉛シート内に侵入することが観察されなかった。黒鉛化ポリイミドシードは、4,4’−ジアミノジフェニルエーテルおよびピロメリト酸二無水物から得たポリイミドフィルムから作製された。
評価に用いたサンプルを表2に示す。ピロメリト酸二無水物と4,4’−ジアミノジフェニルエーテルとの重合によって作製したポリイミドを、PI黒鉛として用いた。異なる厚みを有し、天然の黒鉛のシートを含んでいる5種類の黒鉛のシート、および3M社(3M Company)から入手した市販品(Nextel 312 フレームストッピングドットペーパー)を用いた。
黒鉛フィルムの熱伝導率は、以下の式(1)に従って計算することができる:
λ=α×d×Cp (1)。
光学的な交流通電法に用いられる熱拡散率測定器(アルバック株式会社(ULVAC Inc.)から入手可能なレーザピット(LaserPit))を用いて熱拡散率を決定した。黒鉛フィルムから4×40mmのサンプルを切り出し、このサンプルを、20℃の大気中において10Hzにて分析した。
京都電子工業株式会社(Kyoto Electronics Manufacturing Co., Ltd)製のLFA−502を用いて、レーザフラッシュ法によって、厚み方向における黒鉛フィルムの熱拡散率および熱導電率を、日本工業規格(JIS)R1611−1997に従って測定した。黒鉛フィルムを10mmの直径になるように切り出し、タスコジャパン株式会社(Tasco Japan Co. Ltd.)製の黒体スプレーを、このフィルムの両側に向かって噴霧した。厚み方向における熱拡散率は、室温にてレーザフラッシュ法を用いて測定した。
黒鉛フィルムの密度を、黒鉛フィルムの重量(g)を体積(cm3)で除することによって計算した。体積は、黒鉛フィルムの長さ、幅、および厚みを乗ずることによって得た。黒鉛フィルムの厚みは、50mm×50mmのフィルムの任意の10箇所の厚みを、膜厚計(ハイデンハイン(Heidenhain)製のハイデンハイン−セルト(HEIDENHAIN−CERTO))を用いて、25℃の恒温室において測定し、厚みの平均値を求めることによって決定した。密度がより高いということは、黒鉛化の程度がより高いことを意味する。
黒鉛フィルムの比熱容量は、示差走査熱量計DSC220CU(エスアイアイナノテクノロジー株式会社(SII NanoTechnology Inc.)製の熱解析システム)を用いて、窒素気流下において10℃/minの速度にて20℃〜260℃の温度を評価することによって測定した。
導電率を四端子法によって測定した。特に、3mm×6mmの大きさの堅固な黒鉛を作製し、光学顕微鏡を用いてサンプルを観察してサンプル中に破損やしわが無いことを確認した後、外部電極を、銀ペーストを用いて2つの末端に形成し、そして内部電極を、銀ペーストを用いて外部電極間に形成した。定電流発生器(ケースレーインスツルメンツ株式会社(Keithley Instruments Inc.)製、「プログラマブルカレントソース(programmable current source)220」)を用いて、外部電極間に1mAの定電流を流し、電圧計(ケースレーインスツルメンツ株式会社製、ナノボルトメーター(Nano Voltometer)181)を用いて内部電極間の電圧を測定した。(流れた電流/電圧の測定値)×(内部電極間の距離/サンプルの断面積)という式に値を代入することによって導電率を計算した。
フィルムの吸水率を以下のようにして測定した。フィルムを100℃にて30分間乾燥させ、完全に乾燥させた。そして、厚みが25μmである10cm角のサンプルを作製した。サンプルの重量を測定し、重量をA1とした。厚みが25μmである10cm角のサンプルを23℃の蒸留水に24時間浸漬した。その後、サンプルの表面を拭いて水を除去し、すぐに重量を測定した。この重量をA2とした。吸水率を以下の式から決定した:
吸水率(%)=(A2−Al)/Al×100。
シングルユニットおよび複合体の形態の黒鉛フィルムの引張強度および引張モジュラスを、東京精機製作所(Toyo Seiki Seisaku-sho, Ltd.)製のStrograph VESlDを用いて、ASTM−D−882に従って測定した。チャック間の距離が100mmであり、引張速度が室温において50mm/minであるという条件にて測定を3回行い、平均値を用いた。
黒鉛フィルムに対してMIT耐折強さ試験を行った。黒鉛フィルムを1.5×10cmに切り出した。切り出した黒鉛フィルムを、東京精機株式会社(Toyo Seiki Co.)製のMIT耐折強さ試験機タイプD(MIT Folding Endurance Tester Type D)を用いて、試験荷重が100gf(0.98N)であり、速度が90回/minであり、曲げ半径Rが1mmであるという試験に供した。曲げ角度は、左右に対して90°であった。
黒鉛フィルムの酸素透過率を、GTRテック株式会社(GTR Tec Corporation)製のGTR−20XAFKを用いて測定した。ヤナコテクニカルサイエンス株式会社(Yanako Technical Science Inc.)製のG2700Tを用いて、ガスクロマトグラフィーを行った。ヘリウムガスをキャリアガスとして使用し、試験ガス(酸素)の流量が39.2ml/minであり、温度が25℃であり、RHが0%であるという条件にて、(JIS K−7126およびISO 15105−1に従って)等圧法によって測定を行った。測定を5回行い、得られた結果の平均値を用いた。黒鉛フィルムの水素透過性を、GTRテック株式会社製のGTR−20XAFKを用いて測定し、ヤナコテクニカルサイエンス株式会社製のG2700Tを用いてガスクロマトグラフィーを行った。アルゴンガスをキャリアガスとして使用し、試験ガス(水素)の流量が38.5ml/minであり、温度が25℃であり、RHが0%であるという条件にて、(JIS K−7126およびISO 15105−1に従って)等圧法によって測定を行った。測定を5回行い、得られた結果の平均値を用いた。
黒鉛フィルムの示差熱分析を、セイコーインスツルメンツ株式会社(Seiko Instruments Inc.)製のG/DTA−6300(熱重量/示差熱分析計)を用いて、αアルミナを基準として使用し、温度上昇速度が10.0℃/minであり、最大温度が1000℃であるという条件にて行った。図23に示すように0.17%の重量損失が窒素雰囲気下において観察された。図24に示すように、重量損失の変化は窒素雰囲気下においてほとんど観察されなかった。
Claims (26)
- (a)柔軟な黒鉛化ポリマーシートを含む防火障壁システムを調製する工程、および
(b)前記防火障壁システムを構造体に設ける工程
を含み、
前記黒鉛化ポリマーシートのMIT耐折強さが1000回以上である、防火障壁保護材を構造体に設ける方法。 - 前記システムは、感圧性の接着層または粘着層が形成された、黒鉛化ポリマーシートを有する自己接着性構造を含む、請求項1に記載の方法。
- 前記システムは、断熱袋の側面に設けられた、黒鉛化ポリマーシートを含む、請求項1に記載の方法。
- 前記システムは、断熱材料を内部に含むための積層体を含んでおり、
前記積層体は、層の1つとして、柔軟な黒鉛化ポリマーシートを含んでいる、請求項1に記載の方法。 - 前記システムは、断熱ブランケットを含んでおり、
前記断熱ブランケットが、該断熱ブランケットの層の1つとして、柔軟な黒鉛化ポリマーシートを含んでいる、請求項1に記載の方法。 - 前記システムは、積層構造を含んでおり、
前記積層構造が、発泡体の層および防火障壁層を含んでおり、
前記防火障壁層が、柔軟な黒鉛化ポリマーシートである、請求項1に記載の方法。 - 前記システムは、積層構造を含んでおり、
前記積層構造が、無機繊維の層および防火障壁層を含んでおり、
前記防火障壁層が、柔軟な黒鉛化ポリマーシートである、請求項1に記載の方法。 - 前記システムは、積層構造を含んでおり、
前記積層構造が、有機繊維の層および防火障壁層を含んでおり、
前記防火障壁層が、柔軟な黒鉛化ポリマーシートである、請求項1に記載の方法。 - 前記システムは、積層構造を含んでおり、
前記積層構造が、プラスチックの層および防火障壁層を含んでおり、
前記防火障壁層が、柔軟な黒鉛化ポリマーシートである、請求項1に記載の方法。 - 前記プラスチックの層が、繊維によって補強されたプラスチックの層である、請求項9に記載の方法。
- 前記プラスチックの層が、炭素繊維によって補強されたプラスチックの層であり、
前記防火障壁層が、柔軟な黒鉛化ポリマーシートである、請求項9に記載の方法。 - 前記システムは、積層構造を含んでおり、
前記積層構造が、金属シートの層および防火障壁層を含んでおり、
前記防火障壁層が、柔軟な黒鉛化ポリマーシートである、請求項1に記載の方法。 - 前記システムは、積層構造を含んでおり、
前記積層構造が、断熱紙の層および防火障壁層を含んでおり、
前記防火障壁層が、柔軟な黒鉛化ポリマーシートである、請求項1に記載の方法。 - 構造体に設けられる防火障壁システムであって、前記防火障壁システムは、柔軟な黒鉛化ポリマーシートを含み、
前記黒鉛化ポリマーシートのMIT耐折強さが1000回以上である、防火障壁システム。 - 前記黒鉛化ポリマーシートは、
平面方向における熱伝導率が300W/mK以上であり、
厚み方向における熱伝導率が1〜20W/mKであり、かつ
厚み方向における熱伝導率に対する平面方向における熱伝導率の比率が20以上である、
請求項14に記載のシステム。 - 前記黒鉛化ポリマーシートは、ピクチャーフレーム試験において、試験開始後6分にて、3.4W/cm2(3.0BTU/ft2・s)以下のヒートフラックスおよび300℃(527F)以下の温度を示す、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートは、バーンスルー試験において、試験開始後6分にて、3.4W/cm2(3.0BTU/ft2・s)以下のヒートフラックスを示す、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートは、ピクチャーフレーム試験において、試験開始後6分にて、黒鉛の背面側で、8.0W/cm2以下のヒートフラックスを示す、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートは、ピクチャーフレーム試験において、試験開始後6分にて、黒鉛の背面側で、800℃以下の温度を示す、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートの吸水率が、1%以下である、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートの気体透過率が、100.0×106cc/m2・日以下である、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートの電気伝導率が、10000s/cm以上である、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートは、ポリオキサジアゾール、ポリベンゾチアゾール、ポリベンゾビスチアゾール、ポリベンゾオキサゾール、ポリベンゾビスオキサゾール、ポリイミド、ポリアミド、ポリフェニレンベンゾイミダゾール、ポリチアゾール、ポリパラフェニレンビニレン、ポリ(p−フェニレンイソフタルアミド)、ポリ(m−フェニレンベンゾイミダゾール)、およびポリ(フェニレンベンゾビスイミダゾール)からなる群より選ばれるポリマーから調製されたものである、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートは、ポリイミドポリマーから調製されたものである、請求項14に記載のシステム。
- 前記黒鉛化ポリマーシートは、難燃性の接着材料または粘着材料によって、基板またはシステム部材に接着されている、請求項14に記載のシステム。
- 防火障壁保護材を実現する、柔軟な黒鉛化ポリマーシートの利用であって、
前記黒鉛化ポリマーシートのMITが、1000回以上である、黒鉛化ポリマーシートの利用。
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US6952808P | 2008-03-14 | 2008-03-14 | |
US61/069,528 | 2008-03-14 | ||
US19263608P | 2008-09-19 | 2008-09-19 | |
US61/192,636 | 2008-09-19 | ||
PCT/US2009/001592 WO2009114174A2 (en) | 2008-03-14 | 2009-03-13 | Fire barrier protection comprising graphitized films |
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WO2014038023A1 (ja) * | 2012-09-05 | 2014-03-13 | 株式会社大木工藝 | 冷凍庫 |
WO2014124185A1 (en) * | 2013-02-06 | 2014-08-14 | Work Warm Dba Aeris | Breathable insulation for corrosion reduction |
US9730479B2 (en) | 2013-02-06 | 2017-08-15 | Aeris | Insulating apparel |
EP2974774A1 (de) * | 2014-07-15 | 2016-01-20 | HILTI Aktiengesellschaft | Brandschutzband |
JP6435507B2 (ja) | 2014-07-18 | 2018-12-12 | パナソニックIpマネジメント株式会社 | 複合シートとその製造方法および複合シートを用いた電子機器 |
KR101669204B1 (ko) | 2015-04-30 | 2016-10-25 | 에스케이씨 주식회사 | 그라파이트 시트 및 이의 제조방법 |
CN106205904B (zh) * | 2016-06-20 | 2017-06-27 | 河南省亚安绝缘材料厂有限公司 | 一种环保复合绝缘材料 |
WO2019126292A1 (en) * | 2017-12-19 | 2019-06-27 | Dow Global Technologies Llc | Polyurethane or polyisocyanurate foam laminate with aluminum facer and brominated primer layer |
EP3847715A4 (en) * | 2018-09-07 | 2022-04-13 | 3M Innovative Properties Company | FIRE PROTECTION ARTICLES AND RELATED PROCEDURES |
DE102020108932A1 (de) | 2020-03-31 | 2021-09-30 | Kerafol Holding Gmbh | Folienbauteil sowie Verfahren zu dessen Herstellung |
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RU2750367C1 (ru) * | 2020-07-14 | 2021-06-28 | ФЕДЕРАЛЬНОЕ ГОСУДАРСТВЕННОЕ БЮДЖЕТНОЕ УЧРЕЖДЕНИЕ "ВСЕРОССИЙСКИЙ ОРДЕНА "ЗНАК ПОЧЕТА" НАУЧНО-ИССЛЕДОВАТЕЛЬСКИЙ ИНСТИТУТ ПРОТИВОПОЖАРНОЙ ОБОРОНЫ МИНИСТЕРСТВА РОССИЙСКОЙ ФЕДЕРАЦИИ ПО ДЕЛАМ ГРАЖДАНСКОЙ ОБОРОНЫ, ЧРЕЗВЫЧАЙНЫМ СИТУАЦИЯМ И ЛИКВИДАЦИИ ПОСЛЕДСТВИЙ СТИХИЙНЫХ БЕДСТВИЙ" (ФГБУ ВНИИПО МЧС России) | Способ обеспечения пожарной безопасности в обитаемых гермоотсеках космических летательных аппаратов в орбитальном полёте |
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US4935281A (en) * | 1989-04-05 | 1990-06-19 | Springs Industries, Inc. | Flame barrier office building materials |
JP2976481B2 (ja) * | 1989-05-10 | 1999-11-10 | 松下電器産業株式会社 | フィルム状グラファイトの製造方法 |
JPH09182808A (ja) * | 1995-12-28 | 1997-07-15 | Furukawa Techno Material:Kk | 複合耐火シート |
US5985452A (en) * | 1997-03-18 | 1999-11-16 | Ucar Carbon Technology Corporation | Flexible graphite composite sheet and method |
JP3043480U (ja) * | 1997-05-16 | 1997-11-18 | 株式会社石野コーポレーション | バックパネル用防熱パネル |
US6245400B1 (en) * | 1998-10-07 | 2001-06-12 | Ucar Graph-Tech Inc. | Flexible graphite with non-carrier pressure sensitive adhesive backing and release liner |
US6670291B1 (en) * | 2000-10-18 | 2003-12-30 | 3M Innovative Properties Company | Laminate sheet material for fire barrier applications |
AU2003261889A1 (en) * | 2003-09-02 | 2005-03-29 | Kaneka Corporation | Filmy graphite and process for producing the same |
WO2005123582A1 (ja) * | 2004-06-16 | 2005-12-29 | Kaneka Corporation | グラファイトフィルムの製造方法、およびその方法で製造されたグラファイトフィルム |
WO2006057183A1 (ja) * | 2004-11-24 | 2006-06-01 | Kaneka Corporation | グラファイトフィルムの製造方法 |
US8092908B2 (en) * | 2007-05-17 | 2012-01-10 | Kaneka Corporation | Graphite film and graphite composite film |
JP5707039B2 (ja) * | 2007-06-07 | 2015-04-22 | 株式会社カネカ | グラファイト複合フィルム |
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