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TWI858831B - 降低光澤度之聚醯亞胺膜製造方法 - Google Patents

降低光澤度之聚醯亞胺膜製造方法 Download PDF

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TWI858831B
TWI858831B TW112127160A TW112127160A TWI858831B TW I858831 B TWI858831 B TW I858831B TW 112127160 A TW112127160 A TW 112127160A TW 112127160 A TW112127160 A TW 112127160A TW I858831 B TWI858831 B TW I858831B
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polyimide
film
wet film
dianhydride
diamine
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鍾文軒
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達邁科技股份有限公司
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Abstract

本發明係提供一種降低光澤度之聚醯亞胺膜製造方法，其包括有提供提供一二胺單體及一二酸酐單體在溶劑中進行聚合，以形成一聚醯亞胺前驅物溶液，該二胺包括有一4,4'-二胺基二苯醚(4,4'-ODA)佔二胺總莫耳比例10-45%及對苯二胺(p-PDA)佔二胺總莫耳比例90-55%，該二酸酐包括有一均苯四甲酸二酐(PMDA)佔二酸酐總莫耳比例10-50%及一3,3',4,4'-聯苯四羧酸二酐(BPDA)佔二酸酐總莫耳比例90-50%；添加脫水劑及催化劑於該聚醯亞胺前驅物溶液內，並塗佈於一載體上，以形成一聚醯亞胺濕膜，該脫水劑為2-5當量數，該聚醯亞胺濕膜之楊氏模數為230-350Kgf/mm2；提供一壓花輪，於溫度140-200℃，壓力為3~10Kgf/cm2下將該聚醯亞胺濕膜輾壓，使該聚醯亞胺濕膜表面形成凹凸形狀；及將該濕膜進烘烤以形成一60光澤度小於100之聚醯亞胺膜。

Description

降低光澤度之聚醯亞胺膜製造方法
本發明係關於一種降低光澤度之聚醯亞胺膜製造方法，特別係指一種以壓花滾輪輾壓方式於添加脫水劑及催化劑的聚醯亞胺濕膜上形成凹凸表面，再進行加熱乾燥後成為降低光澤度之聚醯亞胺膜者。
可撓性銅箔積層板(Flexible copper clad laminate,FCCL)係廣泛應用於電子產業中作為電路基板(PCB)，FCCL除了具有輕、薄及可撓的優點外，用聚醯亞胺膜還具有電性能及熱性能優良的特點外，其較低的介電常數(Dk)性，使得電信號得到快速的傳遞，良好的熱性能，可使組件易於降溫，較高的玻璃化溫度(Tg)，可使組件在較高的溫度下良好運行。
然而，聚醯亞胺膜通常具有高表面平坦度，使得大多數的入射光線被反射而產生高光澤度。又，高光澤度的聚醯亞胺薄膜，照射於其表面所產生的大量反射光可能會造成視覺上不舒適或長時間觀看時容易使得眼睛疲勞。另外，低光澤度PI膜常用於軟性電路板(flexible printed circuit boards)的基材及覆蓋層(coverlay)等，常用於後段製程進行對位校準，此等軟性電路板廣泛應用於3C產品、光學鏡頭模組、LCD模組等；此外低光澤度可使元件外觀更具有質感與美觀。
一般降低聚醯亞胺膜光澤度之方法，係添加粒子作為消光劑，有增加材料成本的問題之外，添加大量消光劑又會導致聚醯亞胺膜材本身性質易脆裂。
另外有些會直接對聚醯亞胺樹脂進行壓花加工，此種方法通常需要使用已環化完成的聚醯亞胺樹脂經由熱成型方式塑型，如TW201510000A專利中提出由脂環族二胺類與芳香族二酸製備已環化完成聚醯亞胺樹脂於360℃以下溫度條件下製成膜狀型體，再利用壓花加工方式形成具凹凸狀表面。此類熱塑型聚醯亞胺樹脂的機械性質強度通常都較低，在加工成膜後，往往無法達到良好的熱性質與機械性質，在使用上會有諸多不便。
直接在聚醯亞胺濕膜上直接形成凹凸表面，形成降低光澤度之聚醯亞胺膜的方式不僅可以大量減少成本、又不會降低聚醯亞胺膜材本身的機械強度，此方法實為業界可以思考的問題。
本發明係提供一種降低光澤度之聚醯亞胺膜製造方法，其包括有提供二胺單體及一二酸酐單體在溶劑中進行聚合，以形成一聚醯亞胺前驅物溶液，該二胺包括有一4,4'-二胺基二苯醚(4,4'-ODA)佔二胺總莫耳比例10-45%及對苯二胺(p-PDA)佔二胺總莫耳比例90-55%，該二酸酐包括有一均苯四甲酸二酐(PMDA)佔二酸酐總莫耳比例10-50%及一3,3',4,4'-聯苯四羧酸二酐(BPDA)佔二酸酐總莫耳比例90-50%；添加脫水劑及催化劑於該聚醯亞胺前驅物溶液內，並塗佈於一載體上，以形成一聚醯亞胺濕膜，該聚醯亞胺濕膜之楊氏模數為230-350Kgf/mm2；提供一壓花輪，於溫度140-200 ℃，壓力為3~10Kgf/cm2下將該聚醯亞胺濕膜輾壓，使該聚醯亞胺濕膜表面形成凹凸形狀；及將該聚醯亞胺濕膜進烘烤以形成一60光澤度小於100之聚醯亞胺膜。
S1:提供一聚醯亞胺前驅體溶液
S2:將聚醯胺酸溶液塗佈於一載體上，以形成聚醯亞胺濕膜
S3:將該聚醯亞胺濕膜自載體上剝離，進行壓花輪輾壓，以形成凹凸形狀
S4:進行加熱烘烤以形成聚醯亞胺膜
第1圖係本發明降低光擇度之聚醯亞胺膜製造方法之步驟圖。
請參閱第1，本發明低光澤度之聚醯亞胺膜製造方法，其包括有下列步驟。
提供一二胺單體及一二酸酐單體在溶劑中進行聚合，以形成一聚醯亞胺前驅物溶液(S1)，該二胺包括有一4,4'-二胺基二苯醚(4,4'-ODA)佔二胺總莫耳比例10-45%及對苯二胺(p-PDA)佔二胺總莫耳比例90-55%，該二酸酐包括有一均苯四甲酸二酐(PMDA)佔二酸酐總莫耳比例10-50%及一3,3',4,4'-聯苯四羧酸二酐(BPDA)佔二酸酐總莫耳比例90-50%。
添加脫水劑及催化劑於該聚醯亞胺前驅物溶液內，該脫水劑為2-5當量數，並塗佈於一載體上，以形成一濕膜(S2)，該濕膜之楊氏模數為230-350Kgf/mm2。
將濕膜自載體上剝離後，經過具有凹凸形狀及圖騰之壓花輪於溫度140-200℃輾壓，壓力為3~10Kgf/cm2下(S3)，使濕膜表面形成凹凸形狀。
將該濕膜進烘烤以形成一60光澤度小於100之聚醯亞胺膜(S4)。
該溶劑可為非質子性極性溶劑，例如二甲基乙醯胺(DMAC)、N,N'-二甲基甲醯胺(DMF)、N-甲基吡咯啶酮(NMP)、二甲亞碸(DMSO)等。
該脫水劑可為脂肪族酸酐(如醋酸酐及丙酸酐)、芳香族酸酐(如苯酸酐及鄰苯二甲酸酐)等。該催化劑可為雜環三級胺(例如甲吡啶(picoline)、吡啶等)、脂肪族三級胺(例如三乙基胺(TEA)等)、芳香族三級胺(例如二甲苯胺等)等。
以下實施例詳述本發明。
聚醯亞胺前驅體溶液製備
將二胺單體與二酐單體在溶劑下進行聚合，以形成聚醯胺酸，以形成聚醯亞胺前驅體溶液。
聚醯亞胺前驅體溶液A製備：
將二胺單體PDA 4.82克(0.0446莫爾)與ODA 0.99克(0.0050莫爾)以及二酸酐單體PMDA 1.08克(0.0050莫爾)與BPDA 13.11克(0.0446莫爾)攪拌溶於80.00克DMAc溶劑形成20wt%固含量之聚醯亞胺前驅體溶液A。
聚醯亞胺前驅體溶液B製備：
將二胺單體PDA 2.93克(0.0271莫爾)與ODA 4.44克(0.0222莫爾)以及二酸酐單體PMDA 5.38克(0.0246莫爾)與BPDA 7.25克(0.0246莫爾)攪拌溶於80.00克DMAc溶劑形成20wt%固含量之聚醯亞胺前驅體溶液B。
實施例1
取聚醯亞胺前驅體溶液A 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加7.02毫升(2當量)脫水劑與3.61毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤20分鐘形成聚醯亞胺濕膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為140℃，壓花滾輪壓力為3Kgf/cm2，壓花滾輪速度為1M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為89GU之聚醯亞胺膜。
<實施例2>
取聚醯亞胺前驅體溶液A 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加7.02毫升(2當量)脫水劑與3.61毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤20分鐘形成聚醯亞胺濕膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為1M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為76GU之聚醯亞胺膜。
<實施例3>
取聚醯亞胺前驅體溶液B 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加6.99毫升(2當量)脫水劑與3.60毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤20分鐘形成聚醯亞胺濕膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為140℃，壓花滾輪壓力為3Kgf/cm2，壓花滾輪 速度為1M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為95GU之聚醯亞胺膜。
<實施例4>
取聚醯亞胺前驅體溶液B 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加6.99毫升(2當量)脫水劑與3.60毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤20分鐘形成聚醯亞胺濕膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為4M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為82GU之聚醯亞胺膜。
<實施例5>
取聚醯亞胺前驅體溶液A 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加17.55毫升(5當量)脫水劑與3.61毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤15分鐘形成聚醯亞胺濕膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為140℃，壓花滾輪壓力為3Kgf/cm2，壓花滾輪速度為4M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為65GU之聚醯亞胺膜。
<實施例6>
取聚醯亞胺前驅體溶液A 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加17.55毫升(5當量)脫水劑與3.61毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤15分鐘形成聚醯亞胺濕 膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為4M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為59GU之聚醯亞胺膜。
<實施例7>
取聚醯亞胺前驅體溶液B 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加17.47毫升(5當量)脫水劑與3.60毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤15分鐘形成聚醯亞胺濕膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為140℃，壓花滾輪壓力為3Kgf/cm2，壓花滾輪速度為4M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為72GU之聚醯亞胺膜。
<實施例8>
取聚醯亞胺前驅體溶液B 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加17.47毫升(5當量)脫水劑與3.60毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤15分鐘形成聚醯亞胺濕膜；再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為4M/min；再經過350℃烘烤持溫1小時形成具有60光澤度為63GU之聚醯亞胺膜。
比較例1
取聚醯亞胺前驅體溶液A 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加7.02毫升(2當量)脫水劑與3.61毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤20分鐘形成聚醯亞胺濕膜，將聚醯亞胺濕膜自載體或鋼帶上剝離後，再經過350℃烘烤持溫1小時形成具有60光澤度為166GU之聚醯亞胺膜。
比較例2
取聚醯亞胺前驅體溶液A 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，將其塗佈於載體或鋼帶上以80℃烘烤30分鐘形成聚醯亞胺濕膜，再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為1M/min，無法成膜。
比較例3
取聚醯亞胺前驅體溶液A 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加3.51毫升(1當量)脫水劑與3.61毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤20分鐘形成聚醯亞胺濕膜，再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為1M/min，無法成膜。
比較例4
取聚醯亞胺前驅體溶液B 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，將其塗佈於載體或鋼帶上以80℃烘烤30分鐘形成聚醯亞胺濕膜，再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸 面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為1M/min，無法成膜。
比較例5
取聚醯亞胺前驅體溶液B 75克，加入DMAc溶劑25克攪拌稀釋至固含量15wt%，添加3.49毫升(1當量)脫水劑與3.61毫升(1當量)催化劑後，將其塗佈於載體或鋼帶上以80℃烘烤20分鐘形成聚醯亞胺濕膜，再將聚醯亞胺濕膜自載體或鋼帶上剝離後經過具有凹凸面之壓花滾輪輾壓。該壓花滾輪之溫度為200℃，壓花滾輪壓力為10Kgf/cm2，壓花滾輪速度為1M/min，無法成膜。
如上述之實施例與比較例，本發明係在溫度140-200℃，壓力在3-8Kgf/cm2為較佳操作條件。
60度光澤度值測試
依照ASTM D523規範，使用手持式光澤度計(型號為Micro Tri Gloss-BYK Gardner)進行檢測，取3個獨立測量值之平均值。
濕膜楊氏模數測試
將聚醯亞胺濕膜自載體或鋼帶上剝離後，溶劑含量在30wt%下，依照ASTM D882規範，以萬能拉力試驗機(型號為Tinius Olsen 10ST)進行檢測，取5個獨立測量值之平均值。
比較表
Figure 112127160-A0305-02-0011-1
Figure 112127160-A0305-02-0012-2
比較例與實施例的差異說明：
比較例1是成膜後不進行輾壓之聚醯亞胺膜，比較例2是熱閉環的條件下，壓輾後不成膜；比較例3是脫水劑與催化劑不足當量數時的條件下，壓輾後不成膜，與實施例1，2，5，6做比較。
比較例4是熱閉環的條件下，壓輾後不成膜；比較例5是脫水劑與催化劑不足當量數時的條件下，壓輾後不成膜，與實施例3，4，7，8做比較。
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。
S1:提供一聚醯亞胺前驅體溶液
S2:將聚醯胺酸溶液塗佈於一載體上，以形成聚醯亞胺濕膜
S3:將該聚醯亞胺濕膜自載體上剝離，進行壓花輪輾壓，以形成凹凸形狀
S4:進行加熱烘烤以形成聚醯亞胺膜

Claims (4)

  1. 一種降低光澤度之聚醯亞胺膜製造方法，係包括有：提供一二胺單體及一二酸酐單體在溶劑中進行聚合，以形成一聚醯亞胺前驅物溶液，該二胺包括有一4,4'-二胺基二苯醚(4,4'-ODA)佔二胺總莫耳比例10-45%及對苯二胺(p-PDA)佔二胺總莫耳比例90-55%，該二酸酐包括有一均苯四甲酸二酐(PMDA)佔二酸酐總莫耳比例10-50%及一3,3',4,4'-聯苯四羧酸二酐(BPDA)佔二酸酐總莫耳比例90-50%；添加脫水劑及催化劑於該聚醯亞胺前驅物溶液內，該脫水劑為2-5當量數，並塗佈於一載體上，以形成一聚醯亞胺濕膜，該聚醯亞胺濕膜之楊氏模數為230-350Kgf/mm2；提供一壓花輪，於溫度140-200℃，壓力為3~10Kgf/cm2下將該聚醯亞胺濕膜輾壓，使該聚醯亞胺濕膜表面形成凹凸形狀；及將該聚醯亞胺濕膜進烘烤以形成一60光澤度小於100之聚醯亞胺膜。
  2. 如申請專利範圍第1項所述之降低光澤度之聚醯亞胺膜製造方法，其中，該聚醯亞胺濕膜的溶劑含量在20-40%。
  3. 如申請專利範圍第1項所述之降低光澤度之聚醯亞胺膜製造方法，其中，該壓花輪之滾輪速度在1-4M/min。
  4. 如申請專利範圍第1項所述之降低光澤度之聚醯亞胺膜製造方法，其中，該壓花輪係在溫度140-180℃，壓力為3-8Kgf/cm2操作為較佳者。
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