TWI638772B - Polyimide film for calcination graphitization and method for producing graphite film - Google Patents

Polyimide film for calcination graphitization and method for producing graphite film Download PDF

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TWI638772B
TWI638772B TW105139218A TW105139218A TWI638772B TW I638772 B TWI638772 B TW I638772B TW 105139218 A TW105139218 A TW 105139218A TW 105139218 A TW105139218 A TW 105139218A TW I638772 B TWI638772 B TW I638772B
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film
pda
graphite film
oda
diamine
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吳家浩
賴昱辰
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達邁科技股份有限公司
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Abstract

一種用於捲燒式石墨化之聚醯亞胺膜及石墨膜製造方法，該聚醯亞胺膜係包括由二胺及二胺反應而得，該二胺包含4,4'-二胺基二苯醚(4,4'-oxydianiline(4,4'-ODA))及對苯二胺(phenylenediamine(PDA))，其中ODA/PDA之莫耳比為50/50~80/20，二酐為均苯四甲酸二酸酐(pyromellitic dianhydride(PMDA))。該捲筒式石墨膜之製造方法，係將該聚醯亞胺膜進行碳化熱處理，以形成一碳化膜；及將該碳化膜進行石墨化熱處理，以形成一石墨膜。

Description

用於捲燒式石墨化之聚醯亞胺膜及石墨膜製造方法
本發明係關於一種用於捲燒式石墨化之聚醯亞胺膜、石墨膜及其製造方法，特別係指調整聚醯亞胺之組成使其具有適當機械性質，使其碳化膜及石墨膜具有良好的機械強度，避免產生龜裂或斷裂。
行動裝置之快速成長使得輕薄化成為電子產品之趨勢，而電子元件為了縮減體積而讓元件做緊密的堆積，因此晶片、背光模組及電池等的散熱問題成為重要的議題。在導熱、散熱效能要求逐漸嚴峻時，人造軟性石墨膜的問市讓這些問題得以有了解決方案，人造石墨膜具有良好的傳導性、柔軟性及優於銅四倍之熱傳導效率讓石墨膜在行動裝置上被大量地使用。
高導熱石墨膜在製造上係將聚醯亞胺膜經過一串的高溫裂解反應與原子重新排列過程而產生純碳元素，而這些高溫處理過程被稱為碳化與石墨化。碳化過程得主要功能為熱烈解非碳元素，處理溫度約在800-1300℃之間。石墨化的功用則是透過高溫來推動碳原子，使碳原子重新排列而形成連續有序的層狀結構，在過程中會扮隨著發泡的現象，而形成發泡石墨層結構，其操作溫度發生在9500-3000℃間。對所得到的發泡石 墨膜進行軋延處理後可獲得具有柔軟性之石墨膜，以適合於電子設備中之散熱及電磁波遮蔽層。
捲燒製程生產之石墨膜相較片狀或疊狀製程生產之石墨膜具有可省略人工疊片流程的優點，且利於後續製程之連續生產性，大幅降低成本。
唯，習知捲燒式石墨膜之生產，聚醯亞胺膜係成捲曲狀態，在碳化過程容易中容易產生碳化膜脆裂或斷裂，造成良率過低。
本發明係提供一種用於捲燒式石墨化之聚醯亞胺膜及石墨膜製造方法，該聚醯亞胺膜係由二胺化合物及二酐化合物反應而成，藉由調整聚醯亞胺之組成使其具有適當機械性質，使其碳化膜及石墨膜具有良好的機械強度，避免產生龜裂或斷裂。
本發明之聚醯亞胺膜係包括二胺及二酐，該二胺包含4,4'-二胺基二苯醚(4,4'-oxydianiline(4,4'-ODA))、對苯二胺(phenylenediamine(PDA))，二酐為均苯四甲酸二酸酐(pyromellitic dianhydride(PMDA))，其中ODA/PDA之莫耳比為80/20~50/50，與PMDA進行反應所得之聚醯亞胺膜，將該聚醯亞胺膜經過碳化熱處理及石墨化熱處理，而可得到良好機械強度之石墨膜。
21‧‧‧聚醯亞胺膜
22‧‧‧捲筒
23‧‧‧捲筒狀聚醯亞胺膜
請參閱第1圖為本發明捲燒式之石墨膜製造方法之流程圖。
請參閱第2圖為本發明捲燒式之聚醯亞胺膜示意圖。
請參閱第3圖為本發明捲燒式之聚醯亞胺膜剖視圖。
請參閱第1圖為，本發明用於捲燒式石墨化之聚醯亞胺膜及石墨膜製造方法流程圖，步驟一，首先備製一聚醯亞胺膜10(S1)，該聚醯亞胺膜之楊氏模數(Young's modulus)介於330~490Kgf/mm2之間。
該聚醯亞胺膜係由二胺化合物及二酐化合物反應而成，該二胺包含4,4'-二胺基二苯醚(4,4'-oxydianiline(4,4'-ODA))及對苯二胺(phenylenediamine(p-PDA))，其中ODA/PDA之莫耳比為50/50~80/20，二酐為均苯四甲酸二酸酐(pyromellitic dianhydride(PMDA))。
請配合參閱第2圖及第3圖，將聚醯亞胺膜21捲繞於一捲筒22上，以形成一捲筒狀聚醯亞胺膜23(S2)。
將捲筒狀聚醯亞胺膜23於減壓下或氮氣中加熱碳化處理(S3)，其碳化處理溫度為800-1300℃之間，以形成一捲筒狀碳化膜。
將該捲筒狀碳化膜進行加熱石墨化處理(S4)，其加熱溫度為2500-3000℃，以形成良好機械強渡之石墨膜，具有良好的外觀。
以下實施例詳述本發明。
實施例1
製備本發明聚醯亞胺膜。
<實施例1>
聚醯胺酸溶液製備
將80莫耳%之ODA與20莫耳%之PDA溶於與DMAc中，與100莫耳%之PMDA進行反應，獲得20%聚醯胺酸溶液。
聚醯亞胺膜製備
將所獲聚醯胺酸溶液塗佈於鋼帶上，並放入80℃的烘箱內加熱
約30分鐘，以移除大部份的溶劑，而後將上述塗有第一聚醯胺酸溶液之鋼帶放入170℃~370℃的烘箱內，加熱約4小時，並進行雙軸延伸，以形成38、50及75微米之聚醯亞胺膜。
碳化膜備製
將50公尺長之聚醯亞胺膜捲於一石墨材質製捲筒上進行碳化處理，其碳化溫度約為800-1300℃，以形成一捲筒狀碳化膜。
石墨膜製備
將捲筒狀碳化膜進行石墨化製程，其石墨化溫度約為2800℃，以形成發泡石墨膜，再將發泡石墨膜進行延壓，而製成厚度17、25、40微米的石墨膜。
實施例2
重複實施例1之步驟，惟，ODA及PDA之比例為75/25莫耳比，製備38、50及75微米之聚醯亞胺膜，再製成厚度17、25、40微米的石墨膜。
實施例3
重複實施例1之步驟，惟，ODA及PDA之比例為70/30莫耳比，製備25、38、50及75微米之聚醯亞胺膜，再製成厚度10、17、25及40微米的石墨膜。
實施例4
重複實施例1之步驟，唯ODA及PDA之比例為65/35莫耳比， 製備25、38、50微米之聚醯亞胺膜，再製成厚度10、17、25微米的石墨膜。
實施例5
重複實施例1之步驟，惟，ODA及PDA之比例為60/40莫耳比，製備25及38微米之聚醯亞胺膜，再製成厚度10及17微米的石墨膜。
實施例6
重複實施例1之步驟，惟，ODA及PDA之比例為50/50莫耳比，製備25及38微米之聚醯亞胺膜，再製成厚度10及17微米的石墨膜。
實施例7
重複實施例1之步驟，惟，ODA及PDA之比例為40/60莫耳比，製備25及38微米之聚醯亞胺膜，再製成厚度10及17微米的石墨膜。
比較例1
重複實施例1之步驟，惟，ODA及PDA之比例為100/0莫耳比，製備38、50及75微米之聚醯亞胺膜，再製成厚度17、25及40微米的石墨膜。
優：無裂痕
良：小於5處裂痕
差：大於5處裂痕或斷膜
將實施例1~實施例7與比較例1進行比較，相同38微米厚之聚醯亞胺膜製備17微米捲筒式石墨膜，其ODA/PDA莫耳比介於50/50~75/25所得的石墨模具有較佳的外觀。
將實施例1~實施例7進行比較可得知，厚度越薄的石墨膜需以較高PDA比例之聚醯亞胺膜製備方可得到較好的外觀良率。
將實施例1~實施例7進行比較可得知，以同一配比之聚醯亞胺膜製備不同厚度的石墨膜，越薄的石墨膜具有較高的熱擴散係數。
上述特定實施例之內容係為了詳細說明本發明，然而，該等實施例係僅用於說明，並非意欲限制本發明。熟習本領域之技藝者可理解，在不悖離後附申請專利範圍所界定之範疇下針對本發明所進行之各種變化或修改係落入本發明之一部分。

Claims (9)

  1. 一種捲燒式石墨膜之製造方法，其包括有下列步驟：提供一種石墨膜前驅物之捲筒狀聚醯亞胺膜，其厚度為22μm~28μm，其係由二胺及二胺反應而得，該二胺包含4,4'-二胺基二苯醚(4,4'-oxydianiline(4,4'-ODA))及對苯二胺(phenylenediamine(p-PDA))，其中ODA/PDA之莫耳比為40/60~65/35，二酐為均苯四甲酸二酸酐(pyromellitic dianhydride(PMDA))；將該聚醯亞胺膜進行碳化熱處理，以形成一碳化膜；及將該碳化膜進行石墨化熱處理，以形成一石墨膜。
  2. 如申請專利範圍第1項所述之捲燒式石墨膜之製造方法，其中，該聚醯亞胺膜之楊氏模數(Young's modulus)介於330~490Kgf/mm2之間。
  3. 如中請專利範圍第1項所述之捲燒式石墨膜之製造方法，其中，該碳化熱處理溫度在800-1300℃之間。
  4. 如申請專利範圍第1項所述之捲燒式石墨膜之製造方法，其中，該石墨化熱處理溫度在2500-3000℃之間。
  5. 一種捲燒式石墨膜之製造方法，其包括有下列步驟：提供一種石墨膜前驅物之捲筒狀聚醯亞胺膜，其厚度為45μm~85μm，其係由二胺及二胺反應而得，該二胺包含4,4'-二胺基二苯醚(4,4'-oxydianiline(4,4'-ODA))及對苯二胺(phenylenediamine(p-PDA))，其中ODA/PDA之莫耳比為75/25~80/20，二酐為均苯四甲酸二酸酐(pyromellitic dianhydride(PMDA))；將該聚醯亞胺膜進行碳化熱處理，以形成一碳化膜；及 將該碳化膜進行石墨化熱處理，以形成一石墨膜。
  6. 如申請專利範圍第5項所述之捲燒式石墨膜之製造方法，其中，該碳化熱處理溫度在800-1300℃之間。
  7. 如申請專利範圍第5項所述之捲燒式石墨膜之製造方法，其中，該石墨化熱處理溫度在2500-3000℃之間。
  8. 一種用於捲燒式石墨化之聚醯亞胺膜，其厚度為22μm~28μm，其包括有；二胺，該二胺包含4,4'-二胺基二苯醚(4,4'-oxydianiline(4,4'-ODA))及對苯二胺(phenylenediamine(p-PDA))，其中ODA/PDA之莫耳比為40/60~65/35；及二酐，其為均苯四甲酸二酸酐(pyromellitic dianhydride(PMDA))。
  9. 一種用於捲燒式石墨化之聚醯亞胺膜，其厚度為45μm~83μm，其包括有；二胺，該二胺包含4,4'-二胺基二苯醚(4,4'-oxydianiline(4,4'-ODA))及對苯二胺(phenylenediamine(p-PDA))，其中ODA/PDA之莫耳比為75/25~80/20；及二酐，其為均苯四甲酸二酸酐(pyromellitic dianhydride(PMDA))。
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