TWI766488B - 有機高分子薄膜及其製作方法 - Google Patents

有機高分子薄膜及其製作方法 Download PDF

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TWI766488B
TWI766488B TW109145193A TW109145193A TWI766488B TW I766488 B TWI766488 B TW I766488B TW 109145193 A TW109145193 A TW 109145193A TW 109145193 A TW109145193 A TW 109145193A TW I766488 B TWI766488 B TW I766488B
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organic polymer
polymer film
plasma
pulse
substrate
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謝秉諺
張璇玹
陳瑛鴻
何主亮
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逢甲大學
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Priority to CN202111545582.8A priority patent/CN114644770A/zh
Priority to US17/555,289 priority patent/US11969752B2/en
Priority to KR1020210181668A priority patent/KR102641603B1/ko
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Abstract

本發明提供了一種有機高分子薄膜及其製作方法，該有機高分子薄膜主要以下列步驟製成：(A) 提供一二甲苯前驅物以及一基材； (B) 將該基材置於一電漿設備中； (C) 將該電漿設備內進行抽氣，同時引入透過一載流氣體及該載流氣體乘載的該二甲苯前驅物之蒸氣； (D) 開啟該電漿設備，產生一短脈衝電漿；以及 (E) 在該基材上形成該有機高分子薄膜。 其中，該短脈衝電漿之頻率介於1 赫茲（Hz） ~10,000　赫茲（Hz）；該短脈衝電漿之脈衝時間介於1 微秒（μs）~60 微秒（μs）。

Description

有機高分子薄膜及其製作方法
本發明是關於一種有機高分子薄膜及其製作方法，尤指一種可透過二甲苯前驅物和特殊頻率及週期區間的短脈衝電漿，所製備的有機高分子薄膜及其製作方法。
在眾多的有機高分子材料薄膜中，已經發現有許多材料製成的薄膜具有高化學惰性、透明、良好生物相容性、無細胞毒性、高阻水性及高潤滑等特性。因此，類似的薄膜已廣泛於醫療器材、航太及電子工業之中。
普遍來說，具有上述特性的有機高分子材料薄膜，多半可以透過電漿聚合反應為透過有機氣體或是蒸氣。接著，於低壓低溫下進行輝光放電作用而產生電漿化學反應。
電漿聚合反應的主要機制係於接近真空的低壓條件下注入電場，使其內之惰性氣體崩潰而形成電漿。此時電漿空間中之高能電子將會撞擊前驅物氣體分子，使之激發並進行裂解而活化。裂解狀態包含自由電子、陽離子、陰離子及反應性物種自由基，這些極活潑的自由基團將可於低溫下加速化學反應，於氣相或基材表面發生聚合反應而生成薄膜。
前述製作方法的主要特點在於，以巨觀的狀況下來說，製出的薄膜可形成均勻無針孔狀的薄膜。此外，整個製程溫度可達到接近室溫的程度。此外，薄膜組成容易控制，且前驅物限制少並製程彈性高。薄膜的成長速度亦相當迅速。
但是，在傳統電漿聚合反應過程中，由於其電漿放電時間甚長，此連續波高電漿能量之注入會造成大肆破壞分子結構進而產生鍵結，因此所得薄膜通常並非平面結構，相對來說是具有三度空間且不規則排列之高度網狀交聯結構。
上述特性進而造成薄膜在較為精密的應用領域中，容易聚有貼附性不佳的問題。因此目前亟需一種嶄新的製程，來改善相關的問題。
本發明的主要目的，在於解決上述先前技術所提到的需求。據此，本發明提供了一種有機高分子薄膜。該有機高分子薄膜主要透過下列步驟製成。首先，執行步驟(A)，提供一二甲苯前驅物以及一基材。接著，執行步驟(B)，將該基材置於一電漿設備中，再執行步驟(C)，將該電漿設備內進行抽氣，同時引入透過一載流氣體及該載流氣體乘載的該二甲苯前驅物之蒸氣。接著，執行步驟(D)，開啟該電漿設備，產生一短脈衝電漿。最後，執行步驟(E)，在該基材上形成該有機高分子薄膜。其中，該短脈衝電漿之頻率介於1赫茲(Hz)~10,000赫茲(Hz)，而該短脈衝電漿之脈衝時間介於1微秒(μs)~60微秒(μs)。
以上對本發明之簡述，目的在於對本發明之數種面向和技術特徵作一基本說明，發明簡述並非對本發明的詳細表述，因此其目的不在 特別列舉本發明的關鍵性或重要元件，也不是用來界定本發明的範圍，僅為以簡明的方式呈現本發明之數種概念而已。
(A)~(E):步驟
10:二甲苯前驅物
11:脈衝電源供應系統
4:腔體
51:上電極
52:下電極
6:入氣口
7:出氣口
8:基材
9:有機高分子薄膜
圖1係為本發明有機高分子薄膜製作方法實施例之流程圖。
圖2係為本發明實施例電漿設備運作之示意圖。
為能詳細理解本發明的技術特徵及其作用功效，並可根據發明內容據以實現，茲進一步以如圖式所揭露的具體實施例，詳細說明如後。
請同時參照圖1及圖2，圖1係為本發明有機高分子薄膜製作方法實施例之流程圖；圖2係為本發明實施例電漿設備運作之示意圖。
欲製得本實施例之有機高分子薄膜，首先須執行步驟(A)，提供一二甲苯前驅物以及一基材。本實施例步驟(A)所述之二甲苯前驅物10在進入腔體4之前係以液態的的形式存在，當實際上需要開始進行有機高分子薄膜9的製程之前，會先將二甲苯前驅物10升溫或降壓(例如將腔體4抽真空，形成減壓環境)，使二甲苯前驅物10形成蒸氣，藉以引入腔體4內。而本實施例之基材8則可以是高分子材料(Polymer)或金屬。更進一步來說，當本實施例之基材8為高分子材料(Polymer)時，其材質可選自矽膠、橡膠、聚乙烯、聚醚醚酮或其組合。而基材8選用金屬時，可選自不鏽鋼、鈦、鋁或其合金及氧化物所組成的群組，本發明並不加以限制。
更進一步來說，二甲苯前驅物10可以選自鄰二甲基苯(1,2-Dimethylbenzene)、間二甲基苯(1,3-Dimethylbenzene)、對二 甲基苯(1,4-Dimethylbenzene)或其所組成的群組。其中，又以對二甲基苯(1,4-Dimethylbenzene)作為二甲苯前驅物10時，可製得較為優秀的有機高分子薄膜9。
在另一種可能的實施例中，二甲苯前驅物10可以選自鄰二(三氟甲基)苯(1,2-Bis(trifluoromethyl)benzene)、間二(三氟甲基)苯(1,3-Bis(trifluoromethyl)benzene)、對二(三氟甲基)苯(1,4-Bis(trifluoromethyl)benzene)或其組合所組成的群組。其中，又以對二(三氟甲基)苯(1,4-Bis(trifluoromethyl)benzene)作為二甲苯前驅物10時，可製得較為優秀的有機高分子薄膜9。
接著，執行步驟(B)，將該基材置於一電漿設備中。步驟(B)所述的電漿設備即為圖2所示的結構。更精確來說，本實施例之電漿設備主要由腔體4、入氣口6、出氣口7和脈衝電源供應系統11組成。其中入氣口6和出氣口7與腔體4連通，並且脈衝電源供應系統11包含上電極51及下電極52。在本實施例中，脈衝電源供應系統11是選用脈衝電源當作電源供應器。所以本實施例之脈衝電源供應系統11所產生的電漿係以短脈衝波模式進行作用，以低占空比(即低脈衝頻率、短脈衝時間及長熄火時間)之短脈衝電漿以實現本實施例有機高分子薄膜9的的製作。而本實施例之上電極51及下電極52穿過腔體4並設置於腔體4中。基材8即置於下電極52之上。
接著執行步驟(C)，將電漿設備內進行抽氣，同時引入透過一載流氣體及該載流氣體乘載的該二甲苯前驅物之蒸氣。如前述步驟(A)所述，當二甲苯前驅物10受到減壓環境的吸引(因出氣口7抽氣而趨 近真空的腔體4，本實施例之該減壓環境的壓力介於10~10-2托(torr)之間，更佳則可介於10~10-1托(torr)之間)，便會使二甲苯前驅物10的蒸氣沿著入氣口6進入腔體4內。在本實施例中，二甲苯前驅物10的蒸氣係透過載流氣體(基本上本實施例之載流氣體通氣量小於1000標準毫升/分鐘(sccm)，更佳可介於100~200標準毫升/分鐘(sccm)之間)一併乘載進入腔體4中。而本實施例之載流氣體為氬氣(Ar)。
接著，執行步驟(D)，開啟該電漿設備，產生一短脈衝電漿。最後，如步驟(E)一般，在該基材上形成該有機高分子薄膜。本實施例在基材8上形成有機高分子薄膜9主要可因應二甲苯前驅物10的種類不同而有不同的短脈衝電漿參數應用。具體來說，本實施例之短脈衝電漿係以低脈衝頻率及即短脈衝時間之電源波型(即低佔空比之方波，近乎瞬間開啟且伴隨長熄火時間)的形式進行脈衝電源控制。
本實施例所述短脈衝電漿之頻率介於1赫茲(Hz)~10,000赫茲(Hz)，其中最佳為1,000赫茲(Hz)。而脈衝時間介於1微秒(μs)~60微秒(μs)。此外，短脈衝電漿之功率為50瓦(W)。
當二甲苯前驅物10選用對二甲基苯(1,4-Dimethylbenzene)時，選用的短脈衝電漿功率為50瓦(W)，最佳頻率為1,000赫茲(Hz)，脈衝時間最佳為60微秒(μs)。而當二甲苯前驅物10選用對二(三氟甲基)苯(1,4-Bis(trifluoromethyl)benzene)時，選用的短脈衝電漿之功率同樣為50瓦(W)，最佳頻率同樣為1,000赫茲(Hz)，但脈衝時間最佳為20微秒(μs)。
以對二甲基苯(1,4-Dimethylbenzene)作為二甲苯前驅物10產出的有機高分子薄膜9除了具疏水性、較低磨擦係數及抗沾黏特性外，更具有高生物相容性。而選用對二(三氟甲基)苯(1,4-Bis(trifluoromethyl)benzene)作為二甲苯前驅物10產出的有機高分子薄膜9相較於以對二甲基苯(1,4-Dimethylbenzene)作為二甲苯前驅物10產出的有機高分子薄膜9，又具有更高之疏水性及更低之磨擦係數。
綜上所述，雖然本發明已以實施例揭露如上，然其並非用以限定本發明。本發明所屬技術領域中具有通常知識者，在不脫離本發明之精神和範圍的基礎上，當可作各種的更動和潤飾。因此，本發明的保護範圍當視後附的申請專利範圍所界定者為準。
(A)~(E):步驟

Claims (7)

  1. 一種有機高分子薄膜的製作方法，包含：(A)提供一二甲苯前驅物以及一基材；(B)將該基材置於一電漿設備中；(C)將該電漿設備內進行抽氣，同時引入透過一載流氣體及該載流氣體乘載的該二甲苯前驅物之蒸氣；(D)開啟該電漿設備，產生一短脈衝電漿；以及(E)在該基材上形成該有機高分子薄膜；其中，該短脈衝電漿之頻率為1,000赫茲(Hz)；及該短脈衝電漿之功率為50瓦(W)，且其中該短脈衝電漿之脈衝時間為20微秒(μs)或60微秒(μs)。
  2. 如請求項1所述之有機高分子薄膜的製作方法，其中該二甲苯前驅物係選自鄰二甲基苯(1,2-Dimethylbenzene)、間二甲基苯(1,3-Dimethylbenzene)、對二甲基苯(1,4-Dimethylbenzene)或其所組成的群組。
  3. 如請求項1所述之有機高分子薄膜的製作方法，其中該二甲苯前驅物係選自或鄰二(三氟甲基)苯(1,2-Bis(trifluoromethyl)benzene)、間二(三氟甲基)苯(1,3-Bis(trifluoromethyl)benzene)、對二(三氟甲基)苯(1,4-Bis(trifluoromethyl)benzene)或其組合所組成的群組。
  4. 如請求項1所述之有機高分子薄膜的製作方法，其中該基材為高分子材料(Polymer)或金屬。
  5. 如請求項1所述之有機高分子薄膜的製作方法，其中步驟(B)之該電漿設備包含：一腔體；一入氣口，與該腔體連通；一出氣口，與該腔體連通；以及一脈衝電源供應系統，包含一上電極及一下電極，該上電極及該下電極穿過該腔體並設置於該腔體中；其中，該基材置於該下電極上。
  6. 如請求項1所述之有機高分子薄膜的製作方法，其中該載流氣體為氬氣(Ar)。
  7. 一種有機高分子薄膜，係由請求項1所述之有機高分子薄膜的製作方法製作而成。
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