CN108424647A - 一种用于amoled的透明无色聚酰亚胺薄膜、制备方法和amoled装置 - Google Patents
一种用于amoled的透明无色聚酰亚胺薄膜、制备方法和amoled装置 Download PDFInfo
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- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 title claims abstract description 36
- 229920001621 AMOLED Polymers 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229920001721 polyimide Polymers 0.000 claims abstract description 33
- 239000004642 Polyimide Substances 0.000 claims abstract description 30
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000008065 acid anhydrides Chemical class 0.000 claims abstract description 13
- 229960000583 acetic acid Drugs 0.000 claims abstract description 11
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 10
- 150000001412 amines Chemical class 0.000 claims abstract description 6
- 230000009477 glass transition Effects 0.000 claims abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- -1 4,4 '-diaminodiphenyl ethers Chemical class 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 6
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 5
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical group CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 claims description 3
- ITQTTZVARXURQS-UHFFFAOYSA-N 3-methylpyridine Chemical class CC1=CC=CN=C1 ITQTTZVARXURQS-UHFFFAOYSA-N 0.000 claims description 3
- NVKGJHAQGWCWDI-UHFFFAOYSA-N 4-[4-amino-2-(trifluoromethyl)phenyl]-3-(trifluoromethyl)aniline Chemical group FC(F)(F)C1=CC(N)=CC=C1C1=CC=C(N)C=C1C(F)(F)F NVKGJHAQGWCWDI-UHFFFAOYSA-N 0.000 claims description 3
- 125000002619 bicyclic group Chemical group 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- NSGXIBWMJZWTPY-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropane Chemical compound FC(F)(F)CC(F)(F)F NSGXIBWMJZWTPY-UHFFFAOYSA-N 0.000 claims description 2
- FEUISMYEFPANSS-UHFFFAOYSA-N 2-methylcyclohexan-1-amine Chemical class CC1CCCCC1N FEUISMYEFPANSS-UHFFFAOYSA-N 0.000 claims description 2
- NUIURNJTPRWVAP-UHFFFAOYSA-N 3,3'-Dimethylbenzidine Chemical class C1=C(N)C(C)=CC(C=2C=C(C)C(N)=CC=2)=C1 NUIURNJTPRWVAP-UHFFFAOYSA-N 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- AWJUIBRHMBBTKR-UHFFFAOYSA-N isoquinoline Chemical compound C1=NC=CC2=CC=CC=C21 AWJUIBRHMBBTKR-UHFFFAOYSA-N 0.000 claims description 2
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- MHABMANUFPZXEB-UHFFFAOYSA-N O-demethyl-aloesaponarin I Natural products O=C1C2=CC=CC(O)=C2C(=O)C2=C1C=C(O)C(C(O)=O)=C2C MHABMANUFPZXEB-UHFFFAOYSA-N 0.000 description 4
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 2
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- FZZMTSNZRBFGGU-UHFFFAOYSA-N 2-chloro-7-fluoroquinazolin-4-amine Chemical compound FC1=CC=C2C(N)=NC(Cl)=NC2=C1 FZZMTSNZRBFGGU-UHFFFAOYSA-N 0.000 description 1
- YGYCECQIOXZODZ-UHFFFAOYSA-N 4415-87-6 Chemical compound O=C1OC(=O)C2C1C1C(=O)OC(=O)C12 YGYCECQIOXZODZ-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
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- 125000006297 carbonyl amino group Chemical group [H]N([*:2])C([*:1])=O 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- XXKOQQBKBHUATC-UHFFFAOYSA-N cyclohexylmethylcyclohexane Chemical compound C1CCCCC1CC1CCCCC1 XXKOQQBKBHUATC-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
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- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
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- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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Abstract
本发明涉及一种用于AMOLED的透明无色聚酰亚胺(Transparent Polyimide;TPI)材料及其制备方法。所述透明无色聚酰亚胺材料经由聚酰亚胺预聚体制备而成的薄膜,其中该透明无色聚酰亚胺预聚体是由胺类及酸酐于冰乙酸下聚合,通过所述聚酰亚胺预聚体进行流延法,再由热亚胺化而得透明无色聚酰亚胺薄膜。本发明制备出高耐热与高机械强度的聚酰亚胺薄膜,其玻璃转化温度不低于300℃,热膨胀系数(CTE)为<30 ppm/℃(100~200℃),机械强度之拉伸强度不低于150MPa,杨式模量不低于4 GPa,可应用作为柔性AMOLED触控基板。
Description
技术领域
本发明涉及聚酰亚胺薄膜,薄膜制备方法和AMOLED装置,具体是一种提高透明无色聚酰亚胺聚合度用于AMOLED之制备方法。
背景技术
聚酰亚胺是综合性能最佳的有机高分子材料之一。现代发光器件AMOLED的快速发展,需要聚酰亚胺具有较高的热稳定性、较好的机械性能、较高的光学性能。提高这三方面的综合性能对于发光器件(如OLED,AMOLED等)具有重要的作用。目前许多聚酰亚胺薄膜在500nm光线的透过率不到50%,而在 400nm处被100%吸收,整体可见光区域的透光率较低,薄膜呈现深黄色或棕色。另一方面由于单体反应性不佳的关系,造成分子量聚合度偏低,导致其机械性质与热性质较差,无法满足于柔性AMOLED或柔性触控需求。
为了获得高透光的聚酰亚胺薄膜,可以通过控制单体的结构而减少聚合后的聚酰亚胺 分子中电荷转移络合物的形成,从而达到薄膜透明的效果。文献1报道了用4,4′-(六氟异丙烯)二酞酸酐与2,2′-二(三氟甲基)二氨基联苯合成含氟的透明聚酰亚胺薄膜,在450nm处的透光率接近90%,而在400nm处的透光率不到85%,且其热膨胀系数较高,接近了50ppm/℃,当采用均苯四甲酸二酐作为二酐单体,2,2′-二(三氟甲基)二氨基联苯作为二胺单体时,合成得到的聚酰亚胺薄膜的热膨胀系数为3ppm/℃,但400nm处的透光率仅为5%。文献2采用环丁烷四甲酸二酐与2,2′-二(三氟甲基)二氨基联苯聚合得到聚酰亚胺,但膜厚20μm时在450nm处的透光性为85%。文献3公开了一种聚酰亚胺薄膜的制备方法及聚酰亚胺薄膜,聚酰亚胺薄膜树脂的主链结构中引入含酯基团,使树脂主链结构间次价键力作用增强,降低了薄膜热膨胀系数,但是制备方法比较复杂,薄膜的综合性能相对较差。
文献1:Macromolecules, 1991,24(18):5001-5005.
文献2:High Perform.Polym.,2001,13(2): S93-S106.
文献3:CN105175725A。
发明内容
本发明的目的之一是提供一种具有优异光学性并兼顾机械特性及耐热性的透明无色聚酰亚胺薄膜。具体而言,首先提供一种用于AMOLED的透明无色聚酰亚胺薄膜,其采用所述透明无色聚酰亚胺预聚体制备得到,所述透明无色聚酰亚胺预聚体是由胺类与酸酐聚合而得,所述聚酰亚胺预聚体的粘度为3000~5000 mPa·s,固含量为10~20%,所述透明无色聚酰亚胺薄膜的玻璃转化温度不低于300℃,热膨胀系数(CTE)为< 30ppm/℃ (100~200℃),薄膜拉伸强度不低于150MPa,拉伸模量不低于4 GPa。
本发明的目的之二是提供一种具有优异光学性并兼顾机械特性及耐热性的透明无色聚酰亚胺薄膜的制备方法,包括以下步骤:
(1)在有机溶剂中使胺类化合物完全溶解后,
(2)注入选配的催化剂于氮气下均匀搅拌,
(3)再加入酸酐充分聚合反应,得到透明无色聚酰亚胺预聚体
(4)经过流延过程成膜得到产品,
所述选配的催化剂选自2-甲基吡啶、3-甲基吡啶、冰乙酸、异喹啉、吡啶,优选地,冰乙酸。
所述胺类选自2,2'-二(三氟甲基)二氨基联苯、4,4’-二氨基二苯醚、4,4'-二胺基二环己基甲烷 、4,4'-亚甲基双(2-甲基环己胺) 、2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷、3,3'-二甲基联苯胺、双[4-(4-氨基苯氧基)苯基]砜,优选包含10mol%~90mol%的2,2'-二(三氟甲基)二氨基联苯。
所述酸酐选自1,2,3,4-环丁四羧二酐、双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸二酐、4,4'-(六氟亚异丙基)邻苯二甲酸酐、4,4'-氧双邻苯二甲酸酐、3,3',4,4'-二苯基砜四羧酸二酸酐、2,2’,3,3’-联苯四羧酸二酐和2,3’,3,4’-联苯四羧酸二酐中的一种或多种。所述胺类化合物与酸酐的摩尔比为0.5~1。
选配的催化剂与酸酐的质量比为1:1-5。
所述聚合反应温度和时间为先在-10℃搅拌2小时,然后回温至25℃并持续搅拌12小时。
本发明的目的之三是提供一种制备透明无色聚酰亚胺薄膜的流延工艺过程。所述流延过程为经过优选的多梯度温度及升降温速率的烘烤条件制备亚胺化程度不低于99%的透明无色聚酰亚胺薄膜。所述优选的多梯度温度升降过程为将湿膜在80-150℃的热风干燥或加热板干燥1小时后放入高温烤箱,或将透明无色聚酰亚胺预聚体及玻璃(或其他塑胶材质)之复合基板放入高温烤箱,将高纯氮气通入高温烤箱,1小时后烤箱内含氧量不高于1000 ppm, 设定温度梯度如下:30分钟升温到120℃,在120℃维持10分钟,再10分钟升温到150℃,在150℃维持10分钟,再10分钟升温到180℃,在180℃维持10分钟,再20分钟升温到300℃,在300℃维持60分钟,再1小时15分钟降温到180℃,再1小时5分钟降温到50℃;所述薄膜烘烤环境内的氧浓度含量为0~1000 ppm,优选为100~1000 ppm。
本发明的目的之四是提供一种AMOLED装置,包括柔性基板和设置在所述柔性基板上的有源驱动有机发光器件,所述柔性基板包括采用权利要求4的方法制备得到的聚酰亚胺薄膜。
本发明取得如下技术效果:
(1)本发明的透明无色聚酰亚胺薄膜,其玻璃转化温度不低于300℃,热膨胀系数(CTE)为<30 ppm/℃(100~200℃),薄膜拉伸强度不低于150 MPa,拉伸模量不低于4 GPa。
(2)该方法通过使用调节催化剂与胺类及酐类的适当配比,尤其是采用冰乙酸作为催化剂,在含氮气反应釜设备进行合成,之后采用阶段式升降温聚合工艺并全程于低含氧量阶段式升降温薄膜烘烤工艺,制备出高耐热、低热膨胀特性的聚酰亚胺薄膜,该方法可优化反应机制,制备出高耐热低热膨胀特性的聚酰亚胺薄膜,可应用作为柔性AMOLED触控的基板。
附图说明
图1为聚酰亚胺预聚体涂布制模的示意图。
具体实施方式
下面通过具体的实施例对本发明进行详细说明,但这些例举性实施方式并非对本发明的实际保护范围构成任何形式的任何限定。
实施例1
(1)将高纯氮气通入5L反应釜,氮气流量需控制在不小于反应釜液面以上体积的热通量。同时加入2556 g的N,N-二甲基乙酰胺(DMAC),然后将反应釜的温度调节为25℃。逐量加入311.07g 的2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷,启动搅拌器,转子速度为100~300rpm,向上述反应釜加入50.4g的冰乙酸作为催化剂,反应釜内持续通入高纯氮气。
(2)反应釜封口后持续搅拌30~60分钟,直至粉末状固体溶解。
(3)在上述混合的溶液中逐步加入148.91g的双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸二酐,先在-10℃下搅拌2小时,然后在回温至25℃并持续搅拌12小时。
(4) 搅拌完成后,得到了固体浓度为15wt%的聚酰亚胺预聚体(PAA)浆料,再将PAA浆料取出置于容器,封口后放置于冷冻箱-20℃存储。进行浆料涂布前,放置于室温中回温。
(5)将回温后的聚酰亚胺预聚体涂布在不锈钢板基板上,涂布湿膜厚度为10~100μm;用150℃的热风干燥1小时后,将薄膜从不锈钢板上剥离,并用针固定在框架上(如图1所示),将带薄膜基板放入高温烤箱。
(6) 将高纯氮气通入高温烤箱,1小时后烤箱内含氧量不高于1000 ppm, 设定温度梯度如下:30分钟升温到120℃,在120℃维持10分钟,再10分钟升温到150℃,在150℃维持10分钟,再10分钟升温到180℃,在180℃维持10分钟,再23分钟升温到250℃,在250℃维持10分钟,再1小时7分钟升温到450℃,在450℃维持20分钟,再1小时15分钟降温到180℃,再1小时5分钟降温到50℃,制得聚酰亚胺薄膜亚胺化不低于99%。其聚酰亚胺结构如式Ⅰ所示:
式Ⅰ。
亚胺化程度可藉由聚酰胺C=O(CONH; 1668cm-1)吸收峰判断其亚胺化程度。
实施例2
(1)将高纯氮气通入5L反应釜,氮气流量需控制在不小于反应釜液面以上体积的热通量。同时加入2299g的N,N-二甲基乙酰胺(DMAC),然后将反应釜的温度调节为25℃。逐量加入192.14g的2,2'-二(三氟甲基)二氨基联苯,启动搅拌器,转子速度为100~300rpm,向上述反应釜加入50.4g的冰乙酸作为催化剂,反应釜内持续通入高纯氮气。
(2)反应釜封口后持续搅拌10分钟,直至粉末状固体溶解。
(3)在上述混合的溶液中加入222.51g的4,4'-(六氟亚异丙基)邻苯二甲酸酐,先在-10℃下搅拌2小时,然后在回温至25℃并持续搅拌12小时。
(4)搅拌完成后,得到了固体浓度为15 wt%的聚酰亚胺预聚体(PAA)浆料,再将PAA浆料取出置于容器,封口后放置于冷冻箱-20℃存储。进行浆料涂布前放置于室温中回温。
(5)将回温后的聚酰亚胺预聚体涂布在玻璃基板上,涂布湿膜厚度为10~100 μm;用80℃热风干燥30分钟后,将含薄膜与玻璃的复合基板放入高温烤箱。
(6) 将高纯氮气通入高温烤箱,1小时后烤箱内含氧量不高于1000 ppm, 设定温度梯度如下:30分钟升温到120℃,在120℃维持10分钟,再10分钟升温到150℃,在150℃维持10分钟,再10分钟升温到180℃,在180℃维持10分钟,再23分钟升温到250℃,在250℃维持10分钟,再1小时7分钟升温到450℃,在450℃维持20分钟,再1小时15分钟降温到180℃,再1小时5分钟降温到50℃,制得聚酰亚胺薄膜亚胺化不低于99%。其聚酰亚胺结构如式Ⅱ所示:
式Ⅱ。
实施例3:
除将实施例2的222.51g的4,4'-(六氟亚异丙基)邻苯二甲酸酐更换为117.66 g 的1,2,3,4-环丁四羧二酐外,以实施例2的类似相同方式而进行了实施例3,制得聚酰亚胺薄膜亚胺化不低于99%。其聚酰亚胺结构如式Ⅲ所示:
式Ⅲ。
对比例1
除将实施例2的冰乙酸更换为2-甲基吡啶外,以实施例2的相同方式而进行了对比例1,制得聚酰亚胺薄膜。
对比例2
除将实施例2的冰乙酸更换为3-甲基吡啶外,以实施例2的相同方式而进行了对比例2,制得聚酰亚胺薄膜。
对比例3
除将实施例2的冰乙酸更换为不加冰乙酸外,以实施例2的相同方式而进行了对比例3,制得聚酰亚胺薄膜。
性能测试试验
上述实施例和对比例经由亚胺化所得透明无色聚酰亚胺薄膜的测试结果见下表1。
表1
由上表可看出:本发明采用冰乙酸明显增加其分子量,进而增强其相关特性,如 (1).高玻璃化转化温度 (2). 低热膨胀特性 (3).高拉伸模量。与此同时也藉由全程低含氧量阶段式升降温薄膜烘烤工艺,不损失其光学特性下制备出透明无色聚酰亚胺薄膜,满足柔性基板的低热膨胀特性要求,特别适合用于柔性AMOLED触控的相关应用。与此同时藉由全程低含氧量阶段式升降温薄膜烘烤工艺。
应当理解,这些实施例的用途仅用于说明本发明而非意欲限制本发明的保护范围。此外,也应理解,在阅读了本发明的技术内容之后,本领域技术人员可以对本发明作各种改动、修改和/或变型,所有的这些等价形式同样落于本申请所附权利要求书所限定的保护范围之内。
Claims (10)
1.一种用于AMOLED的透明无色聚酰亚胺薄膜,其采用所述透明无色聚酰亚胺预聚体制备得到,所述透明无色聚酰亚胺预聚体是由胺类与酸酐聚合而得,所述聚酰亚胺预聚体的粘度为3000~5000 mPa·s,固含量为10~20%,所述透明无色聚酰亚胺薄膜的玻璃转化温度不低于300℃,热膨胀系数(CTE)为< 30ppm/℃ (100~200℃),薄膜拉伸强度不低于150MPa,拉伸模量不低于4 GPa。
2. 根据权利要求1所述的一种用于AMOLED的透明无色聚酰亚胺薄膜,所述胺类选自2,2'-二(三氟甲基)二氨基联苯、4,4’-二氨基二苯醚、4,4'-二胺基二环己基甲烷 、4,4'-亚甲基双(2-甲基环己胺) 、2,2-双[4-(4-氨基苯氧基)苯基]六氟丙烷、3,3'-二甲基联苯胺、双[4-(4-氨基苯氧基)苯基]砜。
3.一种用于AMOLED的透明无色聚酰亚胺薄膜的制备方法,包括以下步骤:
(1)在有机溶剂中使胺类化合物完全溶解后,
(2)注入选配的催化剂于氮气下均匀搅拌,
(3)再加入酸酐充分聚合反应,得到透明无色聚酰亚胺预聚体
(4)经过流延过程成膜得到产品,
所述选配的催化剂选自2-甲基吡啶、3-甲基吡啶、冰乙酸、异喹啉、吡啶。
4.根据权利要求3所述的一种用于AMOLED的透明无色聚酰亚胺薄膜的制备方法,所述酸酐选自1,2,3,4-环丁四羧二酐、双环[2.2.2]辛-7-烯-2,3,5,6-四羧酸二酐、4,4'-(六氟亚异丙基)邻苯二甲酸酐、4,4'-氧双邻苯二甲酸酐、3,3',4,4'-二苯基砜四羧酸二酸酐、2,2’,3,3’-联苯四羧酸二酐和2,3’,3,4’-联苯四羧酸二酐中的一种或多种。
5.根据权利要求3所述的一种用于AMOLED的透明无色聚酰亚胺薄膜的制备方法,所述胺类化合物与酸酐的摩尔比为0.5~1。
6.根据权利要求3所述的一种用于AMOLED的透明无色聚酰亚胺薄膜的制备方法,所述选配的催化剂与酸酐的质量比为1:1-5。
7.根据权利要求3所述的一种用于AMOLED的透明无色聚酰亚胺薄膜的制备方法,所述聚合反应温度和时间为先在-10℃搅拌2小时,然后回温至25℃并持续搅拌12小时。
8.根据权利要求3所述的一种用于AMOLED的透明无色聚酰亚胺薄膜的制备方法,所述透明无色聚酰亚胺预聚体在流延之前的储存及运送环境为-10℃~-30℃,优选为-15℃~-20℃。
9. 根据权利要求4所述的一种用于AMOLED的透明无色聚酰亚胺薄膜的制备方法,所述流延过程为经过梯度升降温的烘烤条件制备亚胺化程度不低于99%的透明无色聚酰亚胺薄膜,所述烘烤在高纯氮气下进行,氧浓度含量为0~1000 ppm,优选为100~1000 ppm。
10.一种AMOLED装置,包括柔性基板和设置在所述柔性基板上的有源驱动有机发光器件,所述柔性基板包括采用权利要求3-9的制备方法得到的透明无色聚酰亚胺薄膜。
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CN109280195B (zh) * | 2018-09-28 | 2021-05-11 | 张家港康得新光电材料有限公司 | 一种聚酰亚胺膜及其制备方法 |
WO2020083497A1 (en) * | 2018-10-25 | 2020-04-30 | Osram Opto Semiconductors Gmbh | Conversion element, radiation-emitting semiconductor device and method for producing a conversion element |
JP2020084183A (ja) * | 2018-11-14 | 2020-06-04 | 達邁科技股▲分▼有限公司 | ポリイミドフィルムの製造方法 |
CN112048063A (zh) * | 2020-09-04 | 2020-12-08 | 吉林奥来德光电材料股份有限公司 | 一种高性能透明聚酰亚胺薄膜及其制备方法 |
CN114702669A (zh) * | 2022-02-22 | 2022-07-05 | 哈尔滨工业大学 | 用于柔性有源矩阵有机发光显示器的无色透明聚酰亚胺膜 |
CN114702669B (zh) * | 2022-02-22 | 2022-11-04 | 哈尔滨工业大学 | 用于柔性有源矩阵有机发光显示器的无色透明聚酰亚胺膜 |
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