TWI483894B - 透明導電元件的製備方法 - Google Patents

透明導電元件的製備方法 Download PDF

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TWI483894B
TWI483894B TW101146224A TW101146224A TWI483894B TW I483894 B TWI483894 B TW I483894B TW 101146224 A TW101146224 A TW 101146224A TW 101146224 A TW101146224 A TW 101146224A TW I483894 B TWI483894 B TW I483894B
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carbon nanotube
nanotube film
polymer substrate
carbon
transparent conductive
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TW201420492A (zh
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Kai-Li Jiang
Qun-Qing Li
Yang Wei
Shou-Shan Fan
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Hon Hai Prec Ind Co Ltd
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Description

透明導電元件的製備方法
本發明涉及一種透明導電元件的製備方法，尤其涉及一種基於奈米碳管的透明導電元件的製備方法。
奈米碳管(Carbon Nanotube,CNT)係一種新型碳材料，1991年由日本研究人員Iijima在實驗室製備獲得(請參見，Helical Microtubules of Graphitic Carbon,Nature,V354,P56~58(1991))。奈米碳管膜因具有良好的導電性和透光性而備受關注。
Baughma等人2005於文獻“Strong,Transparent,Multifunctional,Carbon Nanotube Sheets”Mei Zhang,Shaoli Fang,Anvar A.Zakhidov,Ray H.Baughman,etc..Science,Vol.309,P1215-1219(2005)中揭示了一種透明導電的奈米碳管膜的製備方法。所述奈米碳管膜可從一奈米碳管陣列中拉取製備。該奈米碳管陣列為一生長在一基底上的奈米碳管陣列。然而，所製備的奈米碳管膜的透光度不夠好。
為克服上述問題，申請人於2009年5月22日申請的CN101585533B號專利中揭示了一種透明奈米碳管膜的製備方法，該方法包括以下步驟：從一奈米碳管陣列中拉取一奈米碳管膜，該奈米碳管膜包括複數個奈米碳管基本平行於奈米碳管膜的表面；以及採用鐳 射掃描該奈米碳管膜，使該奈米碳管膜由於部分奈米碳管被氧化而變薄，從而提高其透光度。該方法製備的透明奈米碳管膜可應用於透明電極、薄膜電晶體、觸摸屏等領域。該透明奈米碳管膜使用時設置於一玻璃基底或樹脂基底表面。
然而，該方法通過鐳射掃描處理奈米碳管膜來提高其透光性，效率較低，而且採用鐳射掃描成本較高。
有鑒於此，確有必要提供一種既高效且成本低廉的製備奈米碳管透明導電元件的方法。
一種透明導電元件的製備方法，其包括以下步驟：提供一奈米碳管膜，該奈米碳管膜包括複數個奈米碳管線並排且間隔設置，以及複數個奈米碳管搭接在該相鄰奈米碳管線之間；將該奈米碳管膜設置於一熱塑性聚合物基底表面；加熱軟化該熱塑性聚合物基底；沿垂直於奈米碳管線的方向拉伸該熱塑性聚合物基底和該奈米碳管膜；以及硬化該熱塑性聚合物基底以保持該奈米碳管膜拉伸後的狀態。
一種透明導電元件的製備方法，其包括以下步驟：提供一奈米碳管膜，該奈米碳管膜包括複數個奈米碳管線並排且間隔設置，以及複數個奈米碳管搭接在該相鄰奈米碳管線之間；將該奈米碳管膜設置於一軟化的聚合物基底表面；拉伸該聚合物基底和該奈米碳管膜；以及硬化該聚合物基底以保持該奈米碳管膜拉伸後的狀態。
本發明提供的製備奈米碳管透明導電元件的方法具有以下優點： 其一，通過拉伸該聚合物基底和該奈米碳管膜可以增大奈米碳管膜的面積並提高奈米碳管膜的透光性；其二，通過拉伸該聚合物基底和該奈米碳管膜的方法製備透明導電元件，工藝簡單，成本低廉。
10‧‧‧透明導電元件
100‧‧‧奈米碳管膜
102‧‧‧奈米碳管線
104‧‧‧奈米碳管
106‧‧‧聚合物基底
110‧‧‧固定裝置
圖1為本發明第一實施的透明導電元件的製備方法的工藝流程圖。
圖2為圖1中的奈米碳管膜的局部放大結構示意圖。
圖3為本發明第一實施的奈米碳管膜的掃描電鏡照片。
圖4為本發明第二實施的透明導電元件的製備方法的工藝流程圖。
以下將結合附圖詳細說明本發明實施例提供的奈米碳管透明導電元件的製備方法。
請同時參閱圖1，本發明第一實施例提供一種透明導電元件10的製備方法，具體包括以下步驟：S10，提供一奈米碳管膜100；S20，將該奈米碳管膜100設置於一熱塑性聚合物基底106表面；S30，加熱軟化該熱塑性聚合物基底106；S40，拉伸該熱塑性聚合物基底106和該奈米碳管膜100；以及S50，硬化該熱塑性聚合物基底106。
所述步驟S10中，所述奈米碳管膜100的製備方法具體包括以下步驟：首先，提供一奈米碳管陣列，優選地，該陣列為超順排奈米碳管陣列。
所述奈米碳管陣列的製備方法可為化學氣相沈積法。也可為石墨電極恒流電弧放電沈積法、鐳射蒸發沈積法等。本實施例中，該奈米碳管陣列為一採用化學氣相沈積法製備在矽基底表面的順排奈米碳管陣列。
其次，採用一拉伸工具從所述奈米碳管陣列中拉取獲得一奈米碳管膜100。
所述奈米碳管膜100的製備方法具體包括以下步驟：(a)從上述奈米碳管陣列中選定一定寬度的複數個奈米碳管片斷，本實施例優選為採用具有一定寬度的膠帶接觸奈米碳管陣列以選定一定寬度的複數個奈米碳管片斷；(b)以一定速度沿基本垂直於奈米碳管陣列生長方向拉取該複數個奈米碳管片斷，以形成一連續的奈米碳管膜100。
在上述拉取過程中，該複數個奈米碳管片段在拉力作用下沿拉伸方向逐漸脫離基底的同時，由於凡得瓦(Van Der Waals)力作用，該選定的複數個奈米碳管片斷分別與其他奈米碳管片斷首尾相連地連續地被拉出，從而形成一奈米碳管膜100。本實施例中，該奈米碳管膜100的寬度與奈米碳管陣列所生長的基底的尺寸有關，該奈米碳管膜100的長度不限，可根據實際需求制得。該奈米碳管膜100的厚度與選取的奈米碳管片段有關，其厚度範圍 為0.5奈米~100微米。本發明實施例中，所述奈米碳管膜100的厚度為50奈米。
進一步參閱圖2和圖3，所述奈米碳管膜100包括複數個奈米碳管線102並排且間隔設置，以及複數個的奈米碳管104搭接在該相鄰奈米碳管線102之間。所述奈米碳管線102的延伸方向與該奈米碳管膜100的拉取方向相同。所述奈米碳管線102由複數個首尾相連的奈米碳管組成。所述奈米碳管線102中的奈米碳管基本沿奈米碳管線102的軸向排列延伸，且奈米碳管之間通過凡得瓦力緊密連接。所述奈米碳管線102之間通過凡得瓦力緊密連接。所述奈米碳管線102均勻分佈在奈米碳管膜100中且沿第一方向排列。該第一方向為D1方向。相鄰的奈米碳管線102之間具有複數個奈米碳管104。該奈米碳管104可與至少兩個相互並排設置的奈米碳管線102接觸。可以理解，所述奈米碳管線102之間也可包括複數個首尾相連的奈米碳管104。所述複數個奈米碳管104的延伸方向與所述奈米碳管線102的延伸方向成一夾角α，該夾角α大於零度且小於90度。所述複數個奈米碳管線102和複數個奈米碳管104相互搭接，從而使該奈米碳管膜100中的所有奈米碳管形成一導電網絡。進一步，所述奈米碳管膜100為一自支撐結構。所謂自支撐結構即所述奈米碳管膜100只需部分設置在一支撐體上即可維持其膜狀結構，且奈米碳管膜100本身的結構不會發生變化。例如，將所述奈米碳管膜100設置在一框架或兩個間隔設置的支撐結構上，位於中間未與框架或支撐結構接觸的奈米碳管膜100可懸空設置。
所述奈米碳管膜100的長度、寬度及厚度不限，可根據實際需求 製備。所述奈米碳管膜100的厚度優選為大於等於0.5奈米且小於等於1毫米。所述奈米碳管膜100中的奈米碳管的直徑大於等於0.5奈米且小於等於50奈米。所述奈米碳管的長度為大於等於50微米且小於等於5毫米。
所述奈米碳管膜100在垂直於奈米碳管線102的方向上受力後發生形變。該垂直於奈米碳管線102的方向為D2方向。該D2方向垂直於D1方向。當所述奈米碳管膜100在D2方向上被拉伸時，奈米碳管膜100發生形變，奈米碳管線102之間的距離發生變化。具體地，所述奈米碳管線102之間的距離隨奈米碳管膜100形變率的增加而增大。同時，所述奈米碳管104的延伸方向與所述奈米碳管線102的延伸方向的夾角α變大。可以理解，該夾角α最大為90度。所述奈米碳管膜100在D2方向的形變率小於等於300%。當所述奈米碳管膜100在D2方向的形變太大時，該奈米碳管膜100的整體性會受到破壞，即，該奈米碳管膜100中的奈米碳管無法形成一完整導電網絡，而形成複數個分散的導電通路。所述相鄰的奈米碳管線102之間的距離大於0微米且小於等於50微米。該相鄰的奈米碳管線102之間的距離隨奈米碳管膜100的形變率的增加而增大。
所述奈米碳管膜100在D2方向上的形變率與奈米碳管膜100的厚度及密度有關。所述奈米碳管膜100的厚度及密度愈大，其在D2方向上的形變率愈大。進一步地，所述奈米碳管膜100的形變率與奈米碳管線102之間的奈米碳管104的含量有關。在一定含量範圍內，所述奈米碳管線102之間的奈米碳管104的含量越多，所述奈米碳管膜100在D2方向上的形變率越大。所述奈米碳管膜100在D2 方向上的形變率小於等於300%。本發明實施例中，所述奈米碳管膜100的厚度為50奈米，其在D2方向上的形變率可達到150%。
所述奈米碳管膜100的透光度(光透過比率)與奈米碳管膜100的厚度及密度有關。所述奈米碳管膜100的厚度及密度越大，所述奈米碳管膜100的透光度越小。進一步地，所述奈米碳管膜100的透光度與奈米碳管線102之間的距離及奈米碳管104的含量有關。所述奈米碳管線102之間的距離越大，奈米碳管104的含量越少，則所述奈米碳管膜100的透光度越大。所述奈米碳管膜100的透光度大於等於60%且小於等於95%。本發明實施例中，當奈米碳管膜100的厚度為50奈米時，拉伸前該奈米碳管膜100的透光度為大於等於67%且小於等於82%。當其形變率為120%時，所述奈米碳管膜100的透光度為大於等於84%且小於等於92%。以波長為550奈米的綠光為例，拉伸前所述奈米碳管膜100的透光度為78%，當形變率為120%時，該奈米碳管膜100的透光度可達89%。
所述步驟S20中，所述奈米碳管膜100可以直接設置並貼合在所述熱塑性聚合物基底106的一表面。
可以理解，進一步本實施例還可以將複數個奈米碳管膜100層迭設置於所述熱塑性聚合物基底106同一表面，且該複數個奈米碳管膜100中的奈米碳管線102沿同一方向延伸。進一步，本實施例還可以將複數個奈米碳管膜100分別設置於所述熱塑性聚合物基底106相對的兩個表面，且該複數個奈米碳管膜100中的奈米碳管線沿同一方向延伸。進一步，本實施例還可以將所述奈米碳管膜100設置於兩個層迭設置的熱塑性聚合物基底106之間。
所述熱塑性聚合物基底106為一熱塑性聚合物薄膜，其形狀和大 小不限。所述熱塑性聚合物薄膜的厚度為1微米~2毫米，優選地，所述厚度為100微米~1毫米。所述熱塑性聚合物基底106的材料為聚乙烯(PE)、聚氯乙烯(PVC)、聚四氟乙烯(PTFE)、聚丙烯(PP)、聚苯乙烯(PS)、聚甲基丙烯酸甲酯(PMMA)、聚碳酸酯(PC)、聚對苯二甲酸丁二酯(PBT)、聚醯胺(PA)、聚醚酮(PEK)、聚碸(PS)、聚醚碸(PES)、纖維素酯、熱塑性聚醯亞胺(PI)、聚對苯二甲酸乙二酯(PET)、苯並環丁烯(BCB)、聚醚醯亞胺(PEI)、聚苯醚(PPO)、聚苯硫醚(PPS)以及聚乙酸乙烯酯(PVAC)中的一種或者幾種。本實施例中，所述熱塑性聚合物基底106為一厚度100微米的矩形PET薄膜。
所述步驟S30中，所述加熱軟化該熱塑性聚合物基底106的裝置為金屬雙輥、平板熱壓成型機、熱壓機、平板硫化機或烘箱。所述步驟S30的目的為使該熱塑性聚合物基底106軟化為高彈態。
本實施例中，該步驟採用金屬雙輥實現。該金屬雙輥包括兩個可以沿相反方向旋轉的金屬碾壓輥以及一對金屬碾壓輥進行加熱的裝置。將上述設置有奈米碳管膜100的熱塑性聚合物基底106慢慢通過加熱的金屬雙輥，速度控制在1毫米/分~10米/分。該金屬雙輥的溫度要高於所選的熱塑性聚合物基底106的軟化溫度，目的係使得熱塑性聚合物基底106能夠軟化，與奈米碳管膜100緊密接觸，並將奈米碳管膜100與熱塑性聚合物基底106之間的空氣排除。其中，所述金屬雙輥的溫度與所選用的熱塑性聚合物基底106的材料有關，根據不同的熱塑性聚合物基底106的材料，金屬雙輥的溫度不同。進一步，由於金屬雙輥給所述奈米碳管膜100和熱塑性聚合物基底106施加一壓力，從而使該奈米碳管膜100至少 部分嵌入該軟化的熱塑性聚合物基底106之中。本實施例中，所述熱塑性聚合物基底106為一PET薄膜，所述軟化溫度為15℃~200℃。
可以理解，所述步驟S30也可以在一真空環境下進行。該方法可以更有效的將奈米碳管膜100與熱塑性聚合物基底106之間的空氣排出。
所述步驟S40中，所述拉伸該軟化的熱塑性聚合物基底106和奈米碳管膜100的方向不限，只要該拉力在沿著D2方向上形成一分力即可。優選地，直接沿垂直於奈米碳管線102的方向拉伸該軟化的熱塑性聚合物基底106和奈米碳管膜100。
本實施例中，先通過兩個固定裝置110分別將該熱塑性聚合物基底106平行於奈米碳管線102延伸方向的相對兩邊固定，然後沿著D2方向給該兩個固定裝置110分別施加相反的拉力，從而沿著D2方向拉伸該軟化的熱塑性聚合物基底106。可以理解，採用兩個固定裝置110拉伸的奈米碳管膜100和軟化的熱塑性聚合物基底106，可以確保奈米碳管膜100和軟化的熱塑性聚合物基底106受力均勻。
所述拉力的大小和拉伸速度不限，可根據所要拉伸的奈米碳管膜100和軟化的熱塑性聚合物基底106具體進行選擇。如果拉伸速度太大，則軟化的熱塑性聚合物基底106和奈米碳管膜100容易發生破裂，導致奈米碳管膜100的整體性受到破壞。優選地，所述拉伸速度小於20厘米每秒。本實施例中，所述拉伸速度為5厘米每秒。所述拉伸後的奈米碳管膜100中，複數個奈米碳管線102和複數個奈米碳管104相互搭接，從而使該奈米碳管膜100中的所有奈 米碳管形成一導電網絡。
由於所述奈米碳管膜100固定在所述軟化的熱塑性聚合物基底106上，故在拉力的作用下，隨著所述軟化的熱塑性聚合物基底106被拉伸，該奈米碳管膜100也隨之被拉伸。當所述奈米碳管膜100在D2方向上被拉伸時，奈米碳管線102之間的距離變大，同時，所述奈米碳管104的延伸方向與所述奈米碳管線102的延伸方向的夾角α也變大。其中，拉伸前所述並排設置的奈米碳管線102之間的距離大於0微米且小於10微米，拉伸後並排設置的奈米碳管線102之間的距離最大可達50微米。所述奈米碳管膜100被拉伸後仍維持膜狀結構。所述奈米碳管膜100的形變率小於等於300%，且可基本維持奈米碳管膜100的形態。即所述奈米碳管膜100可在原有尺寸的基礎上增加300%。本實施例中，所述奈米碳管膜100為單層奈米碳管膜，拉伸方向為沿垂直於奈米碳管線102的方向，即D2方向。所述奈米碳管膜100在D2方向上的形變率可達150%。
所述步驟S50中，所述硬化該軟化的熱塑性聚合物基底106的方法為降溫硬化。本實施例中，通過自然冷卻法將上述加熱軟化的熱塑性聚合物基底106降溫至室溫從而硬化以保持該奈米碳管膜100拉伸後的狀態。
請同時參閱圖4，本發明第二實施例提供一種透明導電元件10的製備方法，具體包括以下步驟：S10，提供一奈米碳管膜100；S20，將該奈米碳管膜100設置於一軟化的熱固性聚合物基底106 表面；S30，拉伸該熱固性聚合物基底106和該奈米碳管膜100；以及S40，硬化該熱固性聚合物基底106。
本發明第二實施例提供的透明導電元件10的製備方法與第一實施例提供一種透明導電元件10的製備方法基本相同，其區別在於，所述聚合物基底106為一熱固性聚合物基底，且該奈米碳管膜100設置於兩個熱固性聚合物基底106之間。
所述熱固性聚合物基底106的材料可以為酚醛樹脂、環氧樹脂、雙馬來醯亞胺樹脂、聚苯並惡嗪樹脂、氰酸酯樹脂、聚醯亞胺樹脂和不飽和聚醯樹脂中的一種或者幾種。
所述硬化該熱固性聚合物基底106的方法為加熱硬化。所述加熱硬化的溫度可以根據熱固性聚合物基底106的材料選擇。
本發明實施例提供的透明導電元件的製備方法具有以下優點：其一，通過拉伸該聚合物基底和該奈米碳管膜可以增大奈米碳管膜的面積並提高奈米碳管膜的透光性；其二，通過拉伸該聚合物基底和該奈米碳管膜的方法製備透明導電元件，工藝簡單，成本低廉。
綜上所述，本發明確已符合發明專利之要件，遂依法提出專利申請。惟，以上所述者僅為本發明之較佳實施例，自不能以此限制本案之申請專利範圍。舉凡熟悉本案技藝之人士援依本發明之精神所作之等效修飾或變化，皆應涵蓋以下申請專利範圍內。
10‧‧‧透明導電元件
100‧‧‧奈米碳管膜
102‧‧‧奈米碳管線
104‧‧‧奈米碳管
106‧‧‧聚合物基底
110‧‧‧固定裝置

Claims (14)

  1. 一種透明導電元件的製備方法，其包括以下步驟：提供一奈米碳管膜，該奈米碳管膜包括複數個奈米碳管線並排且間隔設置，以及複數個奈米碳管搭接在該相鄰奈米碳管線之間；將該奈米碳管膜直接設置並貼合於一熱塑性聚合物基底表面；加熱軟化該熱塑性聚合物基底；沿垂直於奈米碳管線的方向拉伸該熱塑性聚合物基底和該奈米碳管膜；以及硬化該熱塑性聚合物基底以保持該奈米碳管膜拉伸後的狀態。
  2. 如請求項第1項所述的透明導電元件的製備方法，所述奈米碳管膜為直接從一奈米碳管陣列中拉取獲得，所述奈米碳管線的延伸方向與該奈米碳管膜的拉取方向相同，所述複數個奈米碳管的延伸方向與所述奈米碳管線的延伸方向成一夾角，且該夾角大於零度小於90度。
  3. 如請求項第1項所述的透明導電元件的製備方法，其中，進一步包括將複數個奈米碳管膜層迭設置於所述熱塑性聚合物基底同一表面，且該複數個奈米碳管膜中的奈米碳管線沿同一方向延伸。
  4. 如請求項第1項所述的透明導電元件的製備方法，其中，進一步包括將複數個奈米碳管膜分別設置於所述熱塑性聚合物基底相對的兩個表面，且該複數個奈米碳管膜中的奈米碳管線沿同一方向延伸。
  5. 如請求項第1項所述的透明導電元件的製備方法，其中，進一步包括將所述奈米碳管膜設置於兩個層迭設置的熱塑性聚合物基底之間。
  6. 如請求項第1項所述的透明導電元件的製備方法，其中，所述熱塑性聚合物基底的材料為聚乙烯、聚氯乙烯、聚四氟乙烯、聚丙烯、聚苯乙烯、 聚甲基丙烯酸甲酯、聚對苯二甲酸乙二酯、聚碳酸酯、聚對苯二甲酸丁二酯、聚醯胺、聚醚酮、聚碸、聚醚碸、熱塑性聚醯亞胺、聚醚醯亞胺、聚苯醚、聚苯硫醚、聚乙酸乙烯酯及聚對苯撐苯並雙惡唑中的一種或者幾種的混合物。
  7. 如請求項第1項所述的透明導電元件的製備方法，其中，所述熱塑性聚合物基底為一熱塑性聚合物薄膜，所述熱塑性聚合物薄膜的厚度為1微米~2毫米。
  8. 如請求項第1項所述的透明導電元件的製備方法，其中，所述加熱軟化該熱塑性聚合物基底的裝置為金屬雙輥、平板熱壓成型機、熱壓機、平板硫化機或烘箱。
  9. 如請求項第1項所述的透明導電元件的製備方法，其中，所述加熱軟化該熱塑性聚合物基底的同時，給所述奈米碳管膜施加一壓力，從而使該奈米碳管膜至少部分嵌入該軟化的熱塑性聚合物基底之中。
  10. 如請求項第1項所述的透明導電元件的製備方法，其中，所述拉伸該熱塑性聚合物基底和該奈米碳管膜的速度小於20厘米每秒。
  11. 如請求項第1項所述的透明導電元件的製備方法，其中，所述奈米碳管膜在垂直於奈米碳管線的方向的形變小於300%。
  12. 如請求項第1項所述的透明導電元件的製備方法，其中，所述拉伸後的奈米碳管膜中的複數個奈米碳管線和複數個奈米碳管相互搭接形成一導電網絡。
  13. 一種透明導電元件的製備方法，其包括以下步驟：提供一奈米碳管膜，該奈米碳管膜包括複數個奈米碳管線並排且間隔設置，以及複數個奈米碳管搭接在該相鄰奈米碳管線之間；將該奈米碳管膜設置於一軟化的聚合物基底表面；拉伸該聚合物基底和該奈米碳管膜；以及 硬化該聚合物基底以保持該奈米碳管膜拉伸後的狀態。
  14. 如請求項第13項所述的透明導電元件的製備方法，其中，所述聚合物基底為一熱固性聚合物基底。
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