CN112358612A - 含偕二氟亚甲基的聚酰亚胺薄膜及其制备方法 - Google Patents
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Abstract
Description
技术领域
本发明涉及一种聚酰亚胺薄膜及其制备方法,特别是一种含偕二氟亚甲基的聚酰亚胺薄膜及其制备方法。
背景技术
聚酰亚胺是含有酰亚胺基团的高分子聚合物,因为其具有优异的机械性能、耐热性、绝缘性、轻量化、柔韧性,广泛应用于微电子和航天领域。在柔性显示行业,聚酰亚胺需要具有高的玻璃化转变温度、良好的柔韧性、耐腐蚀性、低的热膨胀系数CTE(Coefficientof thermal expansion)和优异的透过率等。在比较热门的AMOLED领域,加工过程中柔性基板的温度甚至超过300℃,同时还要求聚酰亚胺基板有较好的尺寸稳定性。但是聚酰亚胺大多数为淡黄色,成为其在微电子领域应用的缺点,造成这种淡黄色的原因是聚酰亚胺分子链内或分子链间形成强烈的电荷转移作用(CT charge transfer interactions)。聚酰亚胺由电子供体(芳香二胺链接)和电子受体(芳香二酐的链接)交替组成,两者之间会产生分子内和分子间强烈的电荷转移作用,造成分子链紧密堆积,在可见光的范围内,聚酰亚胺具有强烈的吸收;若二胺所带基团的供电子能力和二酐所带基团的吸电子能力越强,电荷转移作用就越强烈,合成聚酰亚胺的颜色也就越深。
因为氟原子具有强的负电性,摩尔极化率低,在聚酰亚胺分子结构中引入含氟基团可以降低分子链的堆积,减弱分子链内和分子链间的电荷转移效应,减少聚酰亚胺的光学吸收,提高聚酰亚胺的透明度,还可以提高聚酰亚胺的介电性能,制备无色透明的聚酰亚胺薄膜。
发明内容
本发明的目的之一在于提供一种含偕二氟亚甲基的聚酰亚胺薄膜。以满足柔性显示基板等领域对聚酰亚胺薄膜具有较浅颜色、高耐热性、低热膨胀系数等需求。
本发明的目的之二在于提供该含偕二氟亚甲基的聚酰亚胺薄膜的制备方法
为达到上述目的,本发明采用反应机理:
将二胺加入溶剂完全溶解后,与二酐发生亲核加成反应,得到均匀粘稠的聚酰胺酸。将聚酰胺酸涂覆在玻璃表面,加热脱水发生亚胺化反应,得到含氟聚酰亚胺薄膜。
为达到上述目的,采用如下技术方案:
一种含偕二氟亚甲基的聚酰亚胺,其特征在于该含偕二氟亚甲基的聚酰亚胺的结构式为:
所述的R2为:
一种制备上述的含偕二氟亚甲基的聚酰亚胺薄膜的方法,其特征在于该方法的具体步骤为:
a.将含偕二氟亚甲基的二胺或含偕二氟亚甲基的二胺及不含氟芳香二胺按 (10-1):(0-10)的比例溶于溶剂至完全溶解,再加入芳香二酐,反应6–24小时,得到均匀粘稠的聚酰胺酸;所述的二胺与二酐的摩尔比为:1:(1-1.5);所述的含偕二氟亚甲基的二胺的结构式为:R=H,or CH3;所述的不含氟芳香二胺的结构式为:X=O,CH2或零;
b.将步骤a所得聚酰胺酸,在200~320℃,发生亚胺化反应,得到含偕二氟亚甲基的聚酰亚胺薄膜。
上述的薄膜采用涂覆方式制备得到,所述的涂覆方式有浸涂、旋涂或坡流涂布。
上述的溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮或二甲基亚砜。
本发明所得的薄膜具有高耐热性,玻璃化转变温度在200℃以上,具有高机械强度,拉伸强度最高为36.26MPa,低热膨胀系数最低为14.5μm/(m·℃)。
本发明对反应温度不作限定,若超出范围,属于本技术发明基础上适应性调整,仍属于保护范围内。
所述制备方法,预缩聚过程采用的溶剂为N,N-二甲基甲酰胺,N,N-二甲基乙酰胺,N-甲基吡咯烷酮和二甲基亚砜等,本发明不对溶剂作技术性限定。采用溶剂超出说明范围,或者采用多种溶剂混合,都属于在本技术发明基础上联想到的技术改变,仍然属于保护范围内。
所述的制备方法,预缩聚中加料顺序,加料速度,反应时间等反应条件的改变皆不能实质性改变本技术发明的核心,可能会带来一定程度的效果变化,都是属于本发明基础上的衍生技术,仍然属于本发明保护范围。
本发明采用涂覆方式时采用的基板材质有电子玻璃,普通玻璃,钢板。干燥设备有鼓风烘箱,鼓风干燥箱,真空干燥箱,充氮干燥箱。亚胺化最高温度与不同二胺类化合物二酐类化合物相关。
所述的结构简式中,m,n表示聚合度。在本发明技术中,对聚合度并未做限定性范围。聚合度与二胺二酐的摩尔比、二胺二酐的化学活性、预缩聚的条件,亚胺化升温条件等多因素相关。聚合度的改变并不能改变本发明技术的核心思想。
与现有技术相比,本发明技术具备以下突出优点和显著效果:
1.采用含偕二氟亚甲基的二胺及不含氟芳香二胺(0-2种)与芳香二酐类化合物(1-3 种)聚合,得到的聚酰亚胺薄膜具有较好的热性能,能够承受200℃以上的高温工艺。
2.采用含偕二氟亚甲基的二胺(1种)及不含氟芳香二胺(0-2种)与芳香二酐类化合物(1-3种)聚合,得到的聚酰亚胺薄膜具有较好的机械性能。
3.采用刚性结构含偕二氟亚甲基的二胺(1种)及不含氟芳香二胺(0-2种)与芳香二酐类化合物(1-3种)聚合,分子链紧密堆砌,自由体积小,大幅降低了薄膜的膨胀系数,膨胀系数14.5–33.8μm/(m·℃)。
具体实施方式
以下结合具体实施例对本发明进行进一步的详细描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
实施例1:
在反应器中,加入0.7mmol二胺9,9-二氟-9H-芴-2,7-二胺和0.3mmol二胺4,4'-二氨基二苯醚,再加入溶剂N,N-二甲基甲酰胺1.8mL,开启机械搅拌,控制温度10℃,待二胺完全溶解后,加入1mmol二酐3,3',4,4'-联苯四羧酸二酐,反应溶液粘度逐步提高,氮气保护下反应10h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至200℃,200℃保持0.5h,升温至280℃,280℃保持0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
实施例2:
在反应器中,加入0.5mmol二胺9,9-二氟-9H-芴-2,7-二胺和0.5mmol二胺4,4'-二氨基二苯醚,再加入溶剂N,N-二甲基乙酰胺2.3mL,开启机械搅拌,控制温度30℃,待二胺完全溶解后,加入1mmol二酐4,4’-联苯醚二酐(ODPA),反应溶液粘度逐步提高,氮气保护下反应18h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至 300℃,300℃保持0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
实施例3:
在反应器中,加入0.9mmol二胺9,9-二氟-9H-芴-2,7-二胺和0.1mmol二胺4,4'-二氨基二苯醚,再加入溶剂N-甲基吡咯烷酮1.9mL,开启机械搅拌,控制温度25℃,待二胺完全溶解后,加入1mmol二酐4,4’-联苯醚二酐(ODPA),反应溶液粘度逐步提高,氮气保护下反应12h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至 200℃,200℃保持0.5h,升温至250℃,250℃保持0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
实施例4:
在反应器中,加入1mmol二胺9,9-二氟-9H-芴-2,7-二胺,再加入溶剂二甲基亚砜2.5mL,开启机械搅拌,控制温度50℃,待二胺完全溶解后,加入1mmol二酐六氟二酐(6FDA),反应溶液粘度逐步提高,氮气保护下反应18h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至 200℃,200℃保持0.5h,升温至280℃,280℃保持0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
实施例5:
在反应器中,加入1mmol二胺9,9-二氟-9H-芴-2,7-二胺,再加入溶剂N-甲基吡咯烷酮2.3mL,开启机械搅拌,控制温度40℃,待二胺完全溶解后,加入1mmol 二酐4,4’-联苯醚二酐(ODPA),反应溶液粘度逐步提高,氮气保护下反应18h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至 200℃,200℃保持0.5h,升温至250℃,250℃保持0.5h,升温至320℃,320℃保持 0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
实施例6:
在反应器中,加入0.2mmol二胺9,9-二氟-9H-芴-2,7-二胺和0.8mmol二胺4,4'-二氨基二苯醚,再加入溶剂N-甲基吡咯烷酮2mL,开启机械搅拌,控制温度25℃,待二胺完全溶解后,加入1mmol二酐均苯四甲酸二酐,反应溶液粘度逐步提高,氮气保护下反应24h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至200℃,200℃保持0.5h,升温至250℃,250℃保持0.5h,升温至300℃,300℃保持 0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
实施例7:
在反应器中,加入0.5mmol二胺9,9-二氟-9H-芴-2,7-二胺和0.5mmol二胺4,4'-二氨基二苯醚,再加入溶剂N-甲基吡咯烷酮2.2mL,开启机械搅拌,控制温度25℃,待二胺完全溶解后,加入1mmol二酐均苯四甲酸二酐,反应溶液粘度逐步提高,氮气保护下反应24h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至 200℃,200℃保持0.5h,升温至250℃,250℃保持0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
实施例8:
在反应器中,加入0.2mmol二胺9,9-二氟-9H-芴-2,7-二胺和0.8mmol二胺4,4'-二氨基二苯醚,再加入溶剂N,N-二甲基甲酰胺1.8mL,开启机械搅拌,控制温度50℃,待二胺完全溶解后,加入1mmol二酐3,3',4,4'-联苯四羧酸二酐,反应溶液粘度逐步提高,氮气保护下反应18h,得到聚酰胺酸。
将聚酰胺酸旋涂至洗净的玻璃上,放入高温烘箱。进入亚胺化程序升温,烘箱内30min由室温升至100℃,100℃保持0.5h,升温至150℃,150℃保持0.5h,升温至 200℃,200℃保持0.5h,升温至250℃,250℃保持0.5h,升温至320℃,320℃保持 0.5h,自然冷却至室温,从玻璃基板上剥离得到聚酰亚胺薄膜。
将以上实施例1-8所制备的聚酰亚胺薄膜性能进行测试,包括热性能和机械性能,测试结果如下表所示:
从上表中数据可知,通过本发明提供的方法制备出的含偕二氟亚甲基聚酰亚胺薄膜具有良好的热性能,Tg均大于200℃。所有含偕二氟亚甲基的PI薄膜都具有较高的拉伸模量,PI 5和PI 7的拉伸强度和断裂伸长率优于其他4个含偕二氟亚甲基PI 薄膜,表现出较好的机械性能。
以下内容为对上表中各项数据的测试方法进行说明:
Tg由玻璃化转变温度方法测试:DSC:STA409PC综合热分析仪测定,以10℃/min 的加热温度进行差式扫描量热,在第二次加热过程中测试玻璃化转变温度。
机械性能测试方法:用INSTRON 5943薄膜机械分析仪测定。将裁定好的试样置于夹具中,松紧适宜,以防止试样滑脱和断裂在夹具内。在电脑操作面板处设定试验的参数,如试验速度、试验长度和宽度等参数。
膨胀系数(CTE)用TMA Q400仪器测定,氮气气氛,升温速率为10℃/min,静态牵引力为0.05N。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (4)
3.根据权利要求2所述的方法,其特征在于所述的薄膜采用涂覆方式制备得到,所述的涂覆方式有浸涂、旋涂或坡流涂布。
4.根据权利要求2所述的方法,其特征在于所述的溶剂为N,N-二甲基甲酰胺、N,N-二甲基乙酰胺、N-甲基吡咯烷酮或二甲基亚砜。
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