TW522043B - Meso- and nanotubes - Google Patents
Meso- and nanotubes Download PDFInfo
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- TW522043B TW522043B TW089115159A TW89115159A TW522043B TW 522043 B TW522043 B TW 522043B TW 089115159 A TW089115159 A TW 089115159A TW 89115159 A TW89115159 A TW 89115159A TW 522043 B TW522043 B TW 522043B
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經濟部智慧財產局員工消費合作社印製 522043 A7 B7 五、發明說明(Μ 作為中空纖維之中等或奈米管子者,通常指内徑小於 (Κ 1毫米之管料。 具有小的內徑之管子或中空纖維為習知,尤其被用於 分離之目的,例如用於翳藥的透析;用於氣體之分離或 水液系統之滲透,其如水之處理(見Kirk Othmer之化學 技術百科(Encyclopedia of Chemical Technology)第 4版,第13期,第312-313頁)。此種纖維材料大多製自 聚合物,可Μ於其中存有孔性,亦即有半透膜之性能。 用於分離之中空纖維具有75微米至1毫米之內徑,而每 立方厘米體積有100平方厘米之表面積。 中空纖維之另一用途為微電子,由超導材料製成直徑 約以60微米計之纖維超導體,在其中大量填入由聚合物 製成之中空纖維,在聚合物熱分解之後具備超薄性質 (J.C.W. Cien, H.Rinsdorf等人,Adr· Mater.(先進材 料),2(1990)第 305頁)。 具有小内徑之管子通常用擠押抽紡法製成,一糸列之 擠押抽妨方法載於Kirk-〇thmer之Encyclopedia of Chemical Technology,第 4 版,第 317-322頁。 藉助於擠押抽紡法,中空纖維可製成達到2微米内徑 ,更小內徑之中空纖維則未能K此方法製造。 無中空空間之極薄纖維之製造可K用電纺技術(靜電 抽紡)。此中是對聚合物熔體或聚合物溶液在電場中經 由細管於低壓下擠押。此項技術之根據可查閱諸如EP 0 005 035、 EP 0 095 940 - US 5 024 789或 W0 91/ -3- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------*--訂---------線 (請先閱讀背面之注意事項再填寫本頁) 522043 經濟部智慧財產局員工消費合作社印製 A7 B7_ 五、發明說明(2 ) 01695等專利。藉用電紡法可Μ製成直徑自1〇至300奈 米之實心纖維。然而中空纖維之製造也不能用該項技術。 極小直徑之中空纖維迄今僅用電化學合成為可行,如 在 L. A. Chernozan tonskii 於 Chem· Phys. Lett·(化學物 理通訊)297,257(1998)所述,經由超高分子化學之方 法(S· Demoustier, Champagne等人,Europ· Polym· J,(歐洲聚合物會誌)34,1767, (1998),或用自組薄膜 作為模板(E· Evans等人,Science (科學),第273卷, 1996,第933-995頁)〇MFullerene化學為基礎之碳質 中空纖維(具有由單一捲成之石墨Η製成而為一和多壁 結構之碳質奈米小管(Η由各邊互相凝合之六碳環形成) ;或同心設置的石墨圓筒,均載於例如「F u 1 1 e r e n e與 相關結構」(Fullerenes and related Structures),
Ed· a· Hirsch, Springer Verlag 1999年版,第 189緣 234頁;或 Ν· Grobert, Nachr· Chem· Tech· Lab♦(化 學技術實驗報導)47, ( 1999 )第768-776頁。 然而此僅可用於特別的材料,始能使用適當之技術製 造,亦即未能得到力學和化學上均為穩定之中空纖維。 對於例如氣體分離之許多用途,希望具有細小外徑及 /或内徑之中空纖維,依使用範圍而決定採用之材料。 尤其是各種材料應具備耐熱、耐機械力和耐化學性,依 需要而有多孔結構,可選擇導電體或絕緣物。且由聚合 物、無機物或金屬構成。 本發明之課題因而是提供具有奈米至微米範圍内徑而 -4 ~ 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------ί—訂---------線 (請先閱讀背面之注意事項再填寫本頁) 522043 經濟部智慧財產局員工消費合作社印製 A7 B7_ 五、發明說明(3) 由產業上可用之材料製成之中空纖維。 令人驚奇而發現者,具有所希望尺寸内徑之中空纖維 可以準確地由如聚合物、無機物或金屬等各種材料製成。 本發明之標的為具有自10奈米至50微米内徑和由含金 屬之無機化合物、金屬及/或聚合物等構成外壁之中空 纖維。 依本發明之中空纖維較佳具有自50奈米至20微米之内 徑,特佳者自100奈米至5微米,最佳自100奈米至2 微米,或100奈米至1微米,500奈米至1微米,10奈 米至1微米。或100奈米至500奈米。 中空纖維之長度依使用目的而定,一般約為50微米至若 干毫米或厘米。 壁之強度,亦即中空纖維外壁厚度為可變動而通常為 10至500奈米,較佳為10至1000奈米,特佳為1〇至250 奈米。 依據本發明之中空纖維除極小內徑之外具有一糸列之 特性,適合於在醫藥、電子、觸媒、化學分析、氣體分 離、滲透或光學等範疇之用途。 本發明中空纖維外壁可Μ用不同之材料構成,其如聚 合物、金鼷或含金羼之無機化合物。外壁可以設置一層 此等材料,亦即完全由相同或不同材料所成之層或多層 構成。極小內徑使中空纖維在表面積與體積間有高比例 ,可在500與2,000, 000厘米平方/厘米立方之間,較佳 在5,000至1,000,000厘米平方/厘米立方,特佳者在 -5- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------^—tr---------線 (請先閱讀背面之注音3事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 522043 A7 B7 五、發明說明(4) 5, 000至500, 0000厘米平方/厘米立方之間。 本發明中空纖維所含金鼷無機化合物,例如為金屬氧 化物、金靨混合氧化物、尖晶石、金屬氮化物、金屬硫 化物、金鼷碳化物、金屬鋁酸鹽或鈦酸鹽。硼化合物和 用金屬摻雜之碳質奈米管料,其具有一和多壁之結構而 單一捲製石墨片(片之各例互相凝合之六碳環形成)或同 心設置之石墨圓筒等所構成者,在本發明之情形中不含 金屬之化合物。同樣在本發明情形中不含金屬之化合物 者為與碳質奈米管相似之材料,為具有同心設置之多面 或圓筒之片狀結構者,例如WS 2 、MoS 2和VS 2 。 在本發明中之聚合物為縮聚物、加成聚合化合物或聚 合產物,然而不是由純的或摻雜之碳所成近似石墨之化 合物。 再者為製造本發明標的中空纖維之方法。 製造本發明中空纖維之方法,可K實施於使一纖維獲 自於由第一種可分解材料,且至少有另一材料所成之至 少一塗層所構成,最後該第一種材料比例分解,使所成 中空纖維有自18奈米至50微米之内徑。 本發明之中空纖維可以含有如第Id圖之芯。在本發明 另一實施例中,不分解之材料先後與一第二種可分解材 料和至少另一材料塗層。第二可分解材料依定量分解。 繫於該至少之另一材料,可K得到内徑自1 〇奈米至5 0微 米之中空纖維,具有由第一種材料所成之芯。 本發明有芯之中空纖維具有距外壁為自1 〇至3 0 0奈米 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------—----*—訂---------線 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 522043 A7 B7 五、發明說明(5) 平均距離,並且可以用無機化合物、陶瓷纖維、碳纖維 、聚合物及/或金鼷構成。較佳之材料另再介紹。 在第lb), C)和d)圖中草繪中空纖維之各種可能結構形 狀K及製法。 在一項演進中,由第一種可分解材料製成之纖維(第 lb圖,I)先被塗覆(第lb圖,H)。此纖維可Μ由二種 可被熱、化學、射線化學、物理、生物、利用電漿、超 音波或用溶劑萃取等方法分解之材料構成。纖維之製造 可用電紡技術。 電紡技術之細節可Μ査閲例如D · Η ♦ R e n e k e r , I · Chun;在 Nanotech·(奈米技術),7, 216(1996)。電紡 設備之主要構造參考第la_。 可分解纖維之直徑須與稍後所希望之中空纖維内徑之 大小同級。通常中空纖維之中孔空間大約與可分解纖維 或塗層之直徑枏同。確實尺寸關係於所用材料或其在分 解程序中的變異,並且不難從原始的研究得知。 作為可分解之纖維材料,可採用有機或無機材料,尤 其是聚合物,如聚酯、聚醚、聚烯烴、聚碳酸酯、聚氨 基甲酸酯、天然聚合物、聚交酯、聚甙、聚〇t甲基苯乙 烯及/或聚丙烯腈。電紡技術可進一步製造多成分纖維 ,亦即在不同各層中有不同材料之纖維,或具有一定表 面形態之纖維,亦即表面平滑或多孔之纖維。 由可分解材料所成之纖維或塗層,其表面特性也決定 隨後各塗層之表面形態。如果希望中空纖維有粗糙或微 -7- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------^--訂----------線 (請先閱讀背面之注意事項再填寫本頁) 522043 經濟部智慧財產局員工消費合作社印製 A7 ___B7 五、發明說明(6) 細結構之內壁,可Μ用可分解材料製成之適當粗糙纖維 。粗糙或微綑結構之纖維可Κ用有易蒸發溶劑之聚合物 溶液經過加工而用電紡技術獲得。另也可Κ加入鹽類如 硫酸鈉、金屬奈米粉、導電性聚合物如聚吡咯或石墨而 明顯提高所油紡材料之導電性。 具有至少另一不可分解材料之塗層,可Μ藉由氣相澱 積、電漿聚合或將在熔態或溶液中之材料塗上而完成。 此塗層可以由不同各層和以不同的材料完成而構成中空 纖維之外壁。 此塗層亦即外壁之構造,可Μ藉由例如氣相澱積、刮 塗、旋塗、浸塗、噴塗或電漿澱積,將各種聚合物如 聚(對二甲苯)、聚丙烯醯胺、聚醯亞胺、聚酯、聚烯烴 、聚碳酸酯、聚醯胺、聚醚、聚伸苯基、聚矽烷、聚矽 氧烷、聚苯並咪唑、聚笨並瞎唑、聚噁唑、聚硫化物、 聚酯醯胺、聚伸芳基乙烯基、聚丙交酯、聚醚酮、聚氨 基甲酸酯、聚W、0 r m 〇 c e r e η、聚丙烯酸酯、聚矽麵、 全芳香共聚酯、聚-Ν -乙烯基吡咯烷酮、聚甲基丙烯酸 羥乙酯、聚甲基丙烯酸甲酯、聚對苯二甲酸乙二醇酯、 聚對苯二甲酸丁二醇酯、聚甲基丙烯腈、聚丙烯腈、聚 乙酸乙烯酯、氯丁二烯橡膠、丁納橡膠、聚丁二烯、聚 四氯乙烯、纖維素(改質或未改質)、藻朊酸鹽或骨膠 原),其均聚物或共聚物及/或摻混物等而完成。 可分解之塗層或纖維可Μ進一步用其他材料塗覆,其 為由一或多種單體經由聚合、縮聚或加成聚合而獲得。 —8 一 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------.—訂---------^ AW (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 522043 Α7 Β7 五、發明說明(7) 適合於均質或共聚合、加成或縮合之單體,例如甲基丙 烯酸酯、、苯乙烯、苯乙烯磺酸酯、二異氟酸1 , 6 ~六伸 甲酯(1^1)、二異氰酸4,4’-亞甲基雙環己_(1^01)、笨 甲基二異氰酸4,4’~亞甲基酯(MDI)、1,4 -丁二醇、乙烯 二胺、乙烯、苯乙烯、丁二烯、丁烯-1、丁烯-2、乙烯 醇、丙烯腈、甲基丙烯酸甲酯、氯乙烯、氟化乙烯或對 苯二甲酸。 此塗層亦即中空纖維外壁之構造,可K由週期表之第 la、 lb、 Ea、 lb、 la、 Ib、IVa、IVb、Vb、VIb 、Vllb及/或VIb等族之金屬,或為純金鼷或為合金而構 成。適合之金屬例如為金。鈀、鋁、鉑、銀、鈦、鈷、 釕、鍩、納、鉀、鈣、鋰、釩、鎳、鎢、鉻、錳及/或 矽。塗層可Μ用金屬經由蒸發,或用適當之金屬有機物 經由分解K C V D (化學蒸汽澱積)法而完成。 聚合物塗層材料可Μ進一步帶有官能基如目旨、醯胺、 胺、矽烷基、矽氧烷基、硫醇、羥基、氨基甲酸乙酯基 、氨基甲酸酯基、腈基、C = C -基、C = C -基、鹵化碳酸基 、亞硪基、δϋ基、吡啶基、芳膦基;或離子基如碳酸、 磺酸;或第四胺等。各官能基可以加於中空纖維之内壁 及/或外壁,並以分離或滲透方法改善中空纖維之表面 特性。官能基也可Μ於事後藉由聚合物一類之轉化而作 化學之改善(例如酯之皂化)。 經由適當之官能基化,活性物質如抗生素、麻醉劑、 蛋白劑如胰島素、抗污劑,農用化學品如除草劑或殺菌 -9- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------.--訂---------線 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 522043 Α7 Β7 五、發明說明(8) 劑等等可以逆而固定於中空纖維之内,及/或以恆定濃 度再予媛慢釋出(予以控制或媛慢釋放)。 中空纖維外壁,亦即不分解之其他材料,亦可由玻璃 、玻璃陶瓷、S i Ο X 、鈣鈦礦、陶瓷、氧化鋁或氧化酷, 並從碳化矽、氮化硼、碳Μ及金屬氧化物等任意選出予 Κ構成。對此同樣可用氣相澱積法(CVD或PVD)或用水熱 法。如通式之鈣鈦礦為合用。
LaXYMgO 其中:X = Ca、Sr、B a Y = Ga ^ A 1 (未作化學計算),有氧離子導電性。 可分解材料之分解作用可Μ K熱、化學、射線感應、 生物、光化學等經由電漿、超音波、分解;或經由用溶 劑萃取而完成。在實用上Μ熱分解為可靠。分解條件依 材料而定在100-500 1和0.001毫巴至1巴,尤其為佳者 在0.001至0.1毫巴。經過材料分解所得之中空纖維,其 壁材由塗層材料構成。 如第1 b、c和d圖所示,不同材料之多層可Μ加於纖維 上。如此所得之中空纖維具有不同的内壁和外壁,或者 中空纖維之外由多層所構成。不同之各層可Μ呈現不同 之功能;所Κ内層可Κ具有用於例如色層分析所用之特 別分離特性;而外層具有高度之機械穩定性。 本發明中空纖維之層次擧例如下: 玻璃/金屬 一10- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------.—訂---------線 (請先閱讀背面之注意事項再填寫本頁) 522043 A7 B7 五、發明說明( 物 物璃合 璃合玻聚鼷 玻聚 \ \ 金 \ \ 物物 / 屬璃 合合鼷 金玻聚聚金 經濟部智慧財產局員工消費合作社印製 體物 , 氣合體 於混氣 用於於 為用用 物 作或, 合M; 膜 化 可質隔 機 別介為 無 特存作 之 維儲供 鼷 纖或提 金 空離途 含 中分用 \ 物 物 物 S 之種 物 合屬 合瓷合璃無物此 合 聚金鼷聚陶聚玻或浮。 化 \ \ 金 \ \ \ \ 芯懸化 機 鼷物物瓷 靨物 \ 瓷物璃物有子純 無瓷金合合陶瓷屬金合瓷陶合玻合之粒或 \ 陶金 \ 聚陶 \聚\ 聚明或濾 物 \ \ 物 \ \ 物 \ 物 / 發體過 合鼷瓷合屬鼷合瓷合璃本液之 聚金陶聚金金聚陶聚玻 、質 之陶 \ 聚聚 屬 \ 物 \ \ 金瓷合鼷瓷 含陶聚金陶 是 別 特 析 分 層 色 在 濾 過 之 子 粒 為 作 中 液 於 或 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) -------------------訂----------線| (請先閱讀背面之注意事項再填寫本頁) 522043 Α7 Β7 五、發明說明(1Q) (請先閲讀背面之注意事項再填寫本頁) 中作油水分離;在透析中作為離子交換劑;用於綑胞、 綑菌或病毒等之大小分離;作為人工肺之主要部份;用 於除鹽、脫水或給水;或於推進劑中作為除水濾器。 本發明中空纖維更可以用於感應技術作為溶劑、氣體 。濕氣或生物之感應器;用於毛細管電泳;用於觸媒糸 統;用於掃描感應顯微技術;或在超輕構造中作為材料 ;對玻璃纖維作為強化物;作為隔音或防震之用;作為 結合劑或填充物;在翳藥分離技術中作為控制釋出系統 或藥劑賦配系統;在透析中,作為人工肺、蛋白質儲器 ;或用於綑胞組織工程。 在成衣/紡纖工業中,本發明中空纖維可K在衣物或 睡袋中供保暖之用;在光致變色或熱致變色之衣物中, 在管之内裡將色料埋入;或在管之內裡Μ標記作為標纟能。 經濟部智慧財產局員工消費合作社印製 此外,本發明中空纖維可作電子、光學或能源回收等 用途。從中空纖維可Μ製成絲線、纜索或電容、微機械 (例如用於壓電成形、奈米蠕動泵或用於光可定位之聚 合物之成形)或層間介電質。關於本發明中空纖維之其 他用途為微反應器,例如用於觸媒之反應、模仿反應和 生物反應等;從陽光轉變產生熱(太陽- ex-系統);在 晶片技術中作為撓性裝置;或在顯微技術中作為感應部 份(例如作為頂針或探針而用於掃描探測顯微鏡或S Ν Ο Μ (掃描近場光學顯微鏡裝置)。 本發明中空纖維具有極低之介電常數,而且因此可以 作為介電質,尤其是在電子構件內作為中間層介電質, -12- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) 經濟部智慧財產局員工消費合作社印製 522043 A7 B7_ 五、發明說明(11 ) 例如用於晶片之製造。在新生代晶片之生產中使用更小 的尺寸或更高的貯存密度,具有低介電常數的中間層介 電質至為重要。本發明中空纖維由於每單位容積中含有 高比例的空氣而具有小於4的K D值(D i e n s t k a in a卜傳輸 通路值),較佳小於3 ,更佳小於2 ,而理想狀況小於 1 . 5 〇 中空纖維作為介電質用途者,較佳為採用襯頁或蓆狀 (例如第2或3圖)。 利用本發明中空纖維大的表面積,也可Μ用於燃料電 池、蓄電池、或用於電化學反應。用於此等用途之中空 纖維外壁是用氧離子導體如鈣鈦礦者。在氧化反應時, 當氧氣通過纖維之中空當中,中空纖維能夠反覆沖洗析 出物(例如一種烯烴)。氧化生成物則形成於中空纖維 之外而被引去。 本發明中空纖維可Μ用作觸媒系統,例如由貴金屬如 鉑或鈀製成者,可用於汽車作為除氮觸媒。 由與綑胞相容之材料所製成之本發明中空纖維,或經 適當改質者,可Μ植入或插入於細胞膜,並用於從綑胞 或漿綑胞各成分內,分離及提取或除去新陳代謝產物、 酵素和漿細胞之其他成分,因此被應用於生物藥物之提 煉。Μ下各實施例應為發明之詳细說明,無限制其範圍 之意。 實施例1 Μ電紡法,無添加物,製造聚丙交酯板狀纖維 -1 3 - 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) -------------------„—訂----------線- (請先閱讀背面之注意事項再填寫本頁) 522043 經濟部智慧財產局員工消費合作社印製 A7 B7_ 五、發明說明(12 ) 在如第1圖所示之電紡設備中Μ 3 5 Κ V (仟伏)之電壓, 從5 SJ聚-L -丙交酯在二氯甲烷中之溶液(導電度<1(Γ7微 秒/厘米)抽紡。從基板(玻璃)至細胞先端(直徑 0.3毫米)之距離為10厘米,纖維不另處理而繼鑛利用 。掃描電子顯微鏡之纖維照片如第2圖所示。 實施例2 利用電紡法而有添加物製造聚丙交酯板狀纖維 在如第1 _所示之電紡裝置中,Μ 35仟伏電壓抽紡5% 聚-L-丙交酯及有1.5¾苯甲基三乙基氯化銨之二氯甲烷 溶液(導電度=417微秒/厘米)。自基板(玻璃至小管尖 端(直徑0.3毫米)之距離為10厘米。纖維未另處理而繼 續應用。纖維之掃描電子顯微鏡攝影如第3圖所示 實施例3 用氣相塗覆製造聚(對二甲苯)中空纖維 將實施例1 Μ電紡製成之聚丙交酯板狀纖維置於如第 4圖所示氣相澱積裝置之試驗空間内。繼而Μ 230毫克 為分析純度之[2.2]Paracyclophan蒸發於220 °C / 0♦!毫 巴,並在800C熱解,因而構成聚(對二甲苯)(PPX)於試 驗空間於約2 0 t。此聚(對二甲苯)/聚丙交酯之複合織 物在275^/0.01巴之真空爐中熱處理8小時。聚丙交 酯板狀纖維之分解可用紅外光識法證明(第5圖)。聚 (對二甲苯)中空纖維之構成,具有約2微米-0·1微米之 内徑,可Μ用掃描電子顯微鏡證明(第7 , 8圖)。 Μ此方法製成之聚(對二甲苯)中空纖維在D Κ值為1 . 2 9 -14- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------—----.--訂、---------線 (請先閱讀背面之注咅?事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 522043 Α7 Β7 五、發明說明(13) (空氣=1)時,具有0.15克/厘米立方之密度。K如此之 纖維所成之襯頁佔有約14容積%之聚(對二甲苯)和86容 積%之空氣。 實施例4 藉由K溶液塗覆製造聚醯亞胺中空纖維 K實施例1用電紡法製成之聚丙交酯,浸泡於K 4¾之 聚醯胺基碳酸於水/ D M F /吡啶中之溶液内。在1 5 0 - 2 8 5 °C /0.01毫巴之真空爐內熱處理此聚醯亞胺基碳酸/聚丙 交酯之複合織物9小時。因此聚丙交酯板狀纖維一面被 熱分解而聚醯胺基碳酸在聚醯亞胺內通過。内徑約為1 微米至0.5微米之聚醯亞胺中空纖維之構造可Μ用掃描 電子顯微鏡方法證明(第10圖)。 實施例5 用氣相塗覆製造聚(對二甲苯)/金之中空纖維 在一蒸發裝置中使金成為氣相而塗鍍依實施例2 Μ電 紡法(具有0.8¾苯甲基三乙基氯化銨於二氯甲烷中作為 添加劑)所製成之聚丙交酯板狀纖維。繼將此聚丙交酯 /金之纖維置於如第4圖所示氣相蒸鍍裝置之試樣空間 内。繼將200毫克分析純度之[2.2]Paracyelophan蒸發 於200 °C / 0.1毫巴,並在700 υ熱解,因而在約20 °C時 於試樣空間內構成聚(對二甲苯)。此聚(對二甲苯)/聚 丙交酯複合織物在285 ^/0.01毫巴之真空爐中熱處理 8小時。聚(對二甲苯)/金之中空纖維,焉有約為〇·3 微米之平均內徑,其構成可Μ用掃描電子顯微鏡法證明 -15- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------*—訂----------線 (請先閱讀背面之注意事項再填寫本頁) 522043 A7 B7 五、發明說明( 14 第 圖 對 處 電 描 掃 聚 比 在素 一元 丨用 是 理 苯 甲 子 前 之 層 鍍 金 之 〇 壁測 內檢 維法 纖方 空鏡 中微 丨顯 法 紡 電 % 2 例 施 實 依 鍍 塗 維相 纖氣 空 Κ 中 錯 之使 鋁中 造置 製裝 覆發 6 塗蒸 例相一 施氣在 實用 劑纖 加之 添鋁 為/ 作酯 中交 烷丙 甲聚 氯此 二將 於繼 銨 。 化維 氯纖 基狀 乙板 三酯 基山父 甲丙 苯聚 8¾之 ο成 用製 ( 所
V 時 小 8 理 處 熱 中 爐 空 真 之 巴 毫 Μ 元 可用 造是 構理 其處 ,前 維之 纖鋁 空 。 中> 鋁 之 徑 粒明 均證 平法 米鏡 微微 5 顯 280 子 在為電 於約描 置有掃 維具用 第 圖 。 維 測 纖 檢 空 法 中 方 璃 鏡 玻 微 造 顯 製 子 法 電 覆 描 7 塗 掃例相 比施氣 素實用 用 用 } (劑 2 加 例添 施為 實作 依中 鍍烷 塗甲 相氯 氣二 矽於 化銨 氧化 以氯 中基 置乙 裝三 發基 蒸甲 一 苯 在8% 玻 4 結 /S1熱 _ Ϊ之 六乂 U維" κ内# 聚®狀 ft ^ « 罾真_ 011六乂 之 13 。e丙 * 毫¾ 0^0 狀0檢 板 /οκ 酯°c/可 交 5 法 丙28譜 聚在光 之於TR 成置用 製維利 法纖。 紡之時 電璃小 —------------------訂---------線- (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 中 璃 玻 之 徑 內 均明 平證 米法 微鏡 5 微 ο顯 為子 約電 有描 具掃 〇 用 圖 , 13造 第構 如之 量維 定纖 構空 第 画 結 酯 交 丙 聚 之 物 加 添 無 成 製 。 紡 圖電 意M 示烷 置甲 裝氯 紡二 月 明圖圖 說 ^~- 2 式第第 圖 模 例 施 實 /1 維 纖 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) 經濟部智慧財產局員工消費合作社印製 522043 Α7 Β7 五、發明說明(h) 第3圖用二氯甲烷Μ電紡製成有添加物之聚丙交酯結 模纖維(實施例2 )。 第4圖用於聚(對二甲苯)之氣相澱積裝置之示意圖, 具有a)壓力計,b)蒸發區,c)熱解區,d)壓力計,e)試 樣空間,f )用於起始材料之石英小舟,g )用於壓力調整 之容受器,h )熱解油,i )冷卻阱,k )真空。 第5圖聚(對二甲苯)所塗覆之聚丙交酯結模纖維,在 2 6 5 t / 0 . 0 1巴熱分解之紅外光譜撿測,各時段:b = 0 小時,c = l小時,d = 2小時,e = 3小時,f = 4小時,g = 6 小時;純聚合物聚丙交酯而聚(對二甲苯)=h。 第6圖聚(對二甲苯)中空纖維纖物之照片。 第7圖聚(對二甲苯)中空纖維在除去聚丙交酯結模纖 維後之掃描電子顯微鏡攝影(實施例3 )。 第8圖聚(對二甲苯)中空纖維在除去聚丙交酯結模纖 維後之掃描電子顯微鏡攝影(聚丙交酯結模纖維Μ電紡 由具有0,8$苯甲基三乙基氯化銨之二氯甲烷製成)。 第9圖聚(對二甲苯)中空纖維在除去聚丙交酯結模纖 維之後,Κ掃描電子顯微鏡攝取中空纖維內壁形態之一。 第10圖聚醯亞胺中空纖維在除去聚丙交酯結模纖維之 後,用掃描電子顯微鏡所攝照片(實施例4 )。 第1 1圖附有内部金鍍層之Ρ Ρ X中空纖維在除去聚丙交 酯結模纖維之後,用掃描電子顯微鏡拍攝之照片(實施 例5 ) 〇 第12圖鋁中空纖維在除去聚丙交酯結模纖維之後,用 -17- 本紙張尺度適用中國國家標準(CNS)A4規格(210 X 297公釐) ------------------·--訂---------線 (請先閱讀背面之注意事項再填寫本頁)
Claims (1)
- 522043 六、申專利範圍 第89115159號「具有從奈米至微米內部直徑之空心纖維管 ,及其製造方法」專利案 (91年5月24日修]£) 六、申請專利範圍: 1 . 一種中空纖維,其特徵爲具有自1 0奈米至50微米內 徑和一外壁,而由含金屬無機化合物、聚合物及/或 金屬所構成。 2 .如申請專利範圍第1項之中空纖維, 其中其內徑爲1〇奈米至1微米。 3 .如申請專利範圍第1或2項之中空纖維,其中此中空 纖維之外壁是由聚(對二甲苯)、聚丙烯醯胺、聚醯亞 胺、聚酯、聚烯烴、聚碳酸酯、聚醯胺、聚醚、聚伸 苯基、聚矽烷、聚矽氧烷、聚苯並咪唑、聚苯並噻唑 、聚噁唑、聚硫化物、聚酯醯胺、聚亞芳基伸乙烯基 、聚丙交酯、聚醚酮、聚氨基甲酸酯、聚楓、〇rmoceren 、聚丙烯酸酯、聚矽酮、全芳香共聚酯、聚-N-乙烯基 吡咯烷酮、聚甲基丙烯酸羥乙酯、聚甲基丙烯酸甲酯 、聚對苯二甲酸乙二醇酯、聚對苯二甲酸丁二醇酯、 聚甲基丙烯腈、聚丙烯腈、聚乙酸乙烯酯、氯丁二烯 橡膠、丁鈉橡膠、聚丁二烯、聚四氯乙烯、纖維素( 改質或未改質)、藻朊酸鹽或骨膠原),其均聚物或 共聚物及/或摻混物等所構成。 4 .如申請專利範圍第1或2項之中空纖維,其中中空纖 522043 V n W______ 六、申請專利範圍 維之外壁由週期表中之1 a、ib、rta、itb、ma、瓜 b、IVa、IVb、Vb、VIb、Vlb 及 / 或 vmb 等族之金屬 ,各以純金屬或合金而構成° 5 .如申請專利範圍第1或2項之中空纖維,其中中空纖 維之外壁由玻璃、玻璃陶瓷、S 1 〇2、鈣鈦礦、陶瓷、 氧化銘或氧化锆等所構成。 6 .如申請專利範圍第1項之中空纖維,其中中空纖維之 外壁是以多層構成。 7 .如申請專利範圍第1或6項之中空纖維,其中中空纖 維具有芯心。 8 ,如申請專利範圍第7項之中空纖維,其中芯心至外壁 具有自10至3 00奈米之平均距離。 9 .如申請專利範圍第7項之中空纖維,其中芯心由無機 化合物、陶瓷纖維、碳纖維、聚合物及/或金屬構成 522043 η >x/__ 六、申請專利範圍 弟一種可分解材料,和至少另一種材料所塗覆,而且 第一種可刀知材料依定量被分解,與至少一其他材料 有關,獲得具有自1 〇奈米至5 〇微米內徑和由第一種 材料構成芯心之中空纖維。 1 3 ·如申請專利範圍第u或1 2項之方法,其中其他材料 疋由無機化合物、聚合物及/或金屬構成。 14 ·如申請專利範圍第11或12項之方法,其中其他材料 由聚(對二甲苯)、聚丙烯醯胺、聚醯亞胺、聚酯、聚 烯烴、聚碳酸酯、聚醯胺、聚醚、聚伸苯基、聚矽烷 、聚砂氧院、聚苯並咪π坐、聚苯並嗤哩、聚嚼嗤、聚 硫化物、聚酯醯胺、聚亞芳基伸乙烯基、聚丙交酯、 聚醚酮、聚氨基甲酸酯、聚楓、〇rm〇ceren、聚丙烯酸 醋、聚矽酮、全芳香共聚酯、聚-N_乙烯基吡咯烷酮、 聚甲基丙烯酸經乙酯、聚甲基丙嫌酸甲酯、聚對苯二 甲酸乙二醇酯、聚對苯二甲酸丁二醇酯、聚甲基丙烯 腈、聚丙烯腈、聚乙酸乙烯酯、氯丁二烯橡膠、丁鈉 橡膠、聚丁一烯、聚四氯乙嫌、纖維素(改質或未改 質)、藻朊酸鹽或骨膠原),其均聚物或共聚物及/ 或摻混物等所構成。 1 5 ·如申請專利範圍第1丨或1 2項之方法, 其中其他材料是由週期表內第la、lb、na、Etb 、Ilia、mb、IVa、IVb、Vb、VIb、VDb 及/或 \lb 等 族之金屬,各以純金屬或合金,所構成。 522043 ^__ 六、申請專利範圍 1 6 ·如申請專利範圍第π或1 2項之方法, 其中其他材料是由金屬氧化物、玻璃、玻璃陶瓷、 S1 〇2、鈣鈦礦、陶瓷、氧化鋁、碳化矽、氮化硼、碳 或氧化銷構成。 1 7 .如申請專利範圍第1 1或1 2項之方法,其中其他材料 是由一或多種單體經聚合作用、縮聚作用或加成聚合 作用而獲得。 1 8 .如申請專利範圍第1 3項之方法,其中其他材料是由一 或多種單體經聚合作用、縮聚作用或加成聚合作用而 獲得。 1 9 .如申請專利範圍第1 4項之方法,其中其他材料是由一 或多種單體經聚合作用、縮聚作用或加成聚合作用而 獲得。 2〇 .如申請專利範圍第1 7項之方法,其中其他材料是由丙 烯酸甲酯、苯乙烯、苯乙烯磺酸酯、1,6 -六伸甲基二 異氰酸酯(HDI )、4,4 ’ -伸甲基雙環己酯二異氰酸酯 (HMDI )、4,4 1 -伸甲基雙(苯甲基二異氰酸酯)(MDI )、 1,4 -丁一醇、乙燦二胺、乙儲、苯乙嫌、丁二烯、丁 烯-1、丁烯-2、乙烯醇、丙烯腈、甲基丙烯酸甲酯、 氯乙烯、氟化乙烯及/或對苯二酸酯等經均質聚合成 或共聚合,加成或縮合而獲得。 2 1 .如申請專利範圍第1 1或1 2項之方法,其中可分解材 料之分解是以熱、化學、生物、放射感應、光化學,經 -4 - 522043 1 A ----—____________六、申請專利範圍 由電獎、超音波或用溶劑萃取而實施。 2 2 .如申請專利範圍第1丨或1 2項之方法,其中此中空纖 維被使用作爲氣體、液體或粒子懸浮體等之分離介質 或貯存介質。 2 3 ·如申請專利範圍第丨丨或1 2項之方法,其中此中空纖 維被使用於透析中作爲人工肺、蛋白質貯存器、控制 釋出或藥劑給配系統或在醫藥分離技術中。 2 4 .如申請專利範圍第1 1或1 2頊之方法,其中此中空纖 維被使用於細胞技術中用於在生物醫藥之分離及/或 提煉中’除去新陳代謝物、酵素及細胞漿之其他成分 〇 2 5 ·如申請專利範圍第1 1或1 2項之方法,其中此中空纖 維被使用作爲微反應器或在微電子業中作爲絲線、纜 索或電容器。 26 ·如申請專利範圍第1 1或1 2項之方法,其中此中空纖 維被使用在超輕技術中作爲連結材料、作爲塡料作爲 機械性補強,或在成衣工業中作爲保溫材料。 2 7 .如申請專利範圍第1 1或1 2項之方法,其中此中空纖 維被使用於燃料電池、蓄電池或在電化學反應中。 2 8 .如申請專利範圍第1 1或1 2項之方法,其中此中空纖 維被使用於毛細管電泳、在掃描感應顯微鏡或在觸媒 等系統中。 29 .如申請專利範圍第1 1或1 2項之方法,其中此中空纖 522043 六、申請專利範圍 維被使用作爲介電質。 30 .如申請專利範圍第1 1或1 2項之方法,其中此中空纖 維被使用於晶片製造中作爲中間層介電質。
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FR1511581A (fr) * | 1966-12-06 | 1968-02-02 | Rech S Tech Et Ind S R T I S A | Procédé de fabrication de fibres creuses |
DE2823521A1 (de) * | 1978-05-30 | 1979-12-06 | Deutsche Automobilgesellsch | Wasserstoffpermeationszelle und verfahren zu ihrer herstellung |
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US5011566A (en) * | 1989-03-15 | 1991-04-30 | The United States Of America As Represented By The Secretary Of The Air Force | Method of manufacturing microscopic tube material |
US6194066B1 (en) * | 1991-04-24 | 2001-02-27 | The United States Of America As Represented By The Secretary Of The Air Force | Microscopic tube devices and method of manufacture |
EP1018495B1 (de) * | 1996-01-21 | 2004-05-19 | Klaus Rennebeck | Verfahren zur Herstellung von Mikrohohlfasern aus keramischem Material |
CA2346011C (en) * | 1997-10-10 | 2009-01-20 | Drexel University | Hybrid nanofibril matrices for use as tissue engineering devices |
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- 2000-07-13 ES ES00949327T patent/ES2311467T3/es not_active Expired - Lifetime
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- 2000-07-13 AT AT00949327T patent/ATE403019T1/de not_active IP Right Cessation
- 2000-07-13 US US10/048,163 patent/US6667099B1/en not_active Expired - Fee Related
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ATE403019T1 (de) | 2008-08-15 |
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EP1200653A1 (de) | 2002-05-02 |
US6667099B1 (en) | 2003-12-23 |
WO2001009414A1 (de) | 2001-02-08 |
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