CN110540663A - 聚酰亚胺薄膜的制备方法及显示面板 - Google Patents
聚酰亚胺薄膜的制备方法及显示面板 Download PDFInfo
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Abstract
一种聚酰亚胺薄膜的制备方法及显示面板,该方法包括将芳香族二胺单体溶于极性非质子有机溶剂中,并加入硅烷偶联剂,搅拌均匀以形成均相溶液;向均相溶液中加入二酐单体,二酐单体与芳香族二胺单体发生缩聚反应,得到聚酰胺酸溶液;将聚酰胺酸溶液形成于玻璃基板上,进行干燥,在真空条件下,进行热扣环反应,自然降温至室温,得到聚酰亚胺薄膜。通过在单体阶段引入硅烷偶联剂,利用硅烷偶联剂水解生成的羟基与玻璃基板上的羟基发生脱水反应生成化学键,增强聚酰亚胺与玻璃基板之间的附着力,从而改善因附着力差造成的两种基材分离的问题。
Description
技术领域
本发明涉及显示技术领域,尤其涉及一种聚酰亚胺薄膜的制备方法及显示面板。
背景技术
对于柔性显示屏幕来说,传统的玻璃基板已不能满足柔性对曲率的要求,取而代之的多为塑料基材。但在显示器制作工艺中,部分制程的温度高达350℃,其中LTPS(LowTemperature Poly-silicon,低温多晶硅)制程的温度甚至高达400℃以上,这些对材料的耐热性提出了更高的要求。而聚酰亚胺因玻璃化转变温度可高达400℃以上,同时具有优异的机械性能和尺寸稳定性,因此成为柔性显示器基板的最佳选择。
对于柔性LCD来说,因为仍然需要利用液晶的光学性质来实现显示,因此需要柔性基板具有优良的透过率,传统的黄色聚酰亚胺已不能满足透过率的需求,无色透明聚酰亚胺因其透过率高达90%从而用作柔性基板。无色透明聚酰亚胺材料多由二胺单体和酸酐单体的聚合制备,而多数研究是通过在聚酰亚胺分子链上引入-CF3基团,利用F原子较强的电负性,破坏电子给体和受体之间的电荷转移络合物(CTC),来制备无色透明聚酰亚胺。
由于将柔性材料作为基板,承载能力较弱,会影响最终的制程效果,因此一般将柔性基材附着在硬质基板上,在制程完成后,将柔性基板与硬质基板剥离,但在制备过程中,聚酰亚胺薄膜与基板因附着力差,会引发两种基材分离的风险。
发明内容
本发明提供一种聚酰亚胺薄膜的制备方法及显示面板,以解决现有的在硬质基板上制备聚酰亚胺薄膜时,由于上下基材的附着力较差,导致聚酰亚胺薄膜与硬质基板分离,从而影响聚酰亚胺薄膜的性能问题。
为解决上述问题,本发明提供的技术方案如下:
本发明提供一种聚酰亚胺薄膜的制备方法,包括以下步骤:
步骤S10,将至少一种芳香族二胺单体溶于极性非质子有机溶剂中,并加入硅烷偶联剂,搅拌均匀以形成均相溶液,其中,所述芳香族二胺单体的结构通式如式(1)所示:H2N-R1-NH2 (1);
步骤S20,向所述均相溶液中加入至少一种二酐单体,所述二酐单体与所述芳香族二胺单体发生缩聚反应,得到聚酰胺酸溶液,其中,所述二酐单体的结构通式如式(2)所示:所述聚酰胺酸的结构通式如式(3)所示:n为正整数;
步骤S30,将所述聚酰胺酸溶液形成于玻璃基板上,进行干燥,在真空条件下,进行热扣环反应,自然降温至室温,得到所述聚酰亚胺薄膜,其中,所述聚酰亚胺的结构通式如式(4)所示:
在本发明的一种实施例中,所述R1基团选自以下结构式中的一种:
在本发明的一种实施例中,所述R2基团选自以下结构式中的一种:
在本发明的一种实施例中,在所述步骤S20中,将所述二酐单体分3~8次加入到所述均相溶液中,所述二酐单体与所述芳香族二胺单体在室温下反应8~20小时。
在本发明的一种实施例中,在所述步骤S30中,将所述聚酰胺酸溶液用300~500目的细砂布过滤,涂布到所述玻璃基板上。
在本发明的一种实施例中,干燥温度为20~160摄氏度,干燥时间为4~12小时,所述热扣环反应的温度范围为100~350摄氏度。
在本发明的一种实施例中,在所述步骤S10中,将两种所述芳香族二胺单体溶于极性非质子有机溶剂中,且两种所述芳香族二胺单体的摩尔比例为1:1至1:10。
在本发明的一种实施例中,在所述步骤S20中,向所述均相溶液中加入一种所述二酐单体,且所述二酐单体与两种所述芳香族二胺单体总和的摩尔比为1:0.5~1:1。
在本发明的一种实施例中,在所述步骤S10中,将一种芳香族二胺单体溶于所述极性非质子有机溶剂中;在所述步骤S20中,向所述均相溶液中加入两种二酐单体。
本发明还提供一种显示面板,包括衬底,所述衬底为如上述制备方法制备的聚酰亚胺薄膜。
本发明的有益效果为:本发明通过共聚的方式制备一种透明聚酰亚胺材料,在制备过程中引入了硅烷偶联剂,利用硅烷偶联剂水解后生成的羟基与玻璃基板上的羟基(在固化升温时)发生脱水反应生成化学键,进而利用这种化学键作用来增强聚酰亚胺与玻璃基板之间的附着力,从而改善因附着力差造成的两种基材分离的问题。
附图说明
为了更清楚地说明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单介绍,显而易见地,下面描述中的附图仅仅是发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。
图1为本发明实施例聚酰亚胺薄膜的制备方法的步骤流程图。
具体实施方式
以下各实施例的说明是参考附加的图示,用以例示本发明可用以实施的特定实施例。本发明所提到的方向用语,例如[上]、[下]、[前]、[后]、[左]、[右]、[内]、[外]、[侧面]等,仅是参考附加图式的方向。因此,使用的方向用语是用以说明及理解本发明,而非用以限制本发明。在图中,结构相似的单元是用以相同标号表示。
本发明针对现有的聚酰亚胺薄膜的制备方法,由于子硬质基板上制备聚酰亚胺薄膜时,上下基材的附着力较差,导致聚酰亚胺薄膜与硬质基板分离,从而影响聚酰亚胺薄膜的性能问题,本实施例能够解决该缺陷。
如图1所示,本发明实施例提供一种聚酰亚胺薄膜的制备方法,所述聚酰亚胺的结构通式如通式(4)所示:所述聚酰亚胺由二胺单体和二酐单体发生缩聚反应得到聚酰胺酸,并且向体系中加入硅烷偶联剂,利用硅烷偶联剂水解后与玻璃基板发生反应以形成透明的聚酰亚胺薄膜。硅烷偶联剂水解后生成的羟基,与玻璃基板上的羟基(在固化升温时)发生脱水反应生成化学键,利用这种化学键作用来增强聚酰亚胺与玻璃基板之间的附着力。
对于柔性LCD技术来说,多将柔性基材附着在硬质基板上(如玻璃基板),在制程完成后,将柔性基板与硬质基板剥离。为了避免制程的过程中,聚酰亚胺薄膜与基板因附着力差引发分离的风险,对两种基材之间的附着力会有较高的要求,另外也需要柔性基材具有优良的透过率,因此本发明实施例针对透明聚酰亚胺薄膜与硬质基板的附着力较差的问题做出改进。
本发明实施例采用两步法制备所述聚酰亚胺薄膜,采用两步法首先制备前驱体聚酰胺酸溶液,在聚酰氨酸溶液中加入硅烷偶联剂,制备改性的聚酰胺酸溶液,涂布在玻璃基板上,最后以梯度升温的方式进行热固化制得改性透明聚酰亚胺薄膜,下面详细介绍本发明实施例所述的制备方法。
步骤S10,将至少一种芳香族二胺单体溶于极性非质子有机溶剂中,并加入硅烷偶联剂,搅拌均匀以形成均相溶液,其中,所述芳香族二胺单体的结构通式如式(1)所示:H2N-R1-NH2 (1);
步骤S20,向所述均相溶液中加入至少一种二酐单体,所述二酐单体与所述芳香族二胺单体发生缩聚反应,得到聚酰胺酸溶液,其中,所述二酐单体的结构通式如式(2)所示:所述聚酰胺酸的结构通式如式(3)所示:n为正整数;
步骤S30,将所述聚酰胺酸溶液形成于玻璃基板上,进行干燥,在真空条件下,进行热扣环反应,自然降温至室温,得到所述聚酰亚胺薄膜,其中,所述聚酰亚胺的结构通式如式(4)所示:
所述芳香族二胺单体中的R1基团选自以下结构式中的一种:
所述二酐单体中的R2基团选自以下结构式中的一种:
首先,在惰性气体(例如氮气)保护氛围下,将前述任意两种结构式不同的所述芳香族二胺单体溶于所述极性非质子有机溶剂中,并向其中加入一定量的所述硅烷偶联剂,搅拌均匀后形成所述均相溶液。其中,两种所述芳香族二胺单体的的摩尔比为1:1至1:10。
所述极性非质子有机溶剂为N,N-二甲基乙酰胺、N,N-二甲基甲酰胺、二甲基亚砜或N-甲基吡咯烷酮中的一种。
之后,向所述均相溶液中分3~8次加入同一种所述二酐单体,分批次加入以便于溶液混合均匀,在室温下,反应8至20小时,得到所述聚酰胺酸溶液,其中,所述二酐单体与上述两种所述芳香族二胺单体总和的摩尔比为1:0.5至1:1。
接着,将得到的所述聚酰胺酸溶液用300至500目的纱布过滤掉杂质后涂布到干净的玻璃基板上,在20至160摄氏度下,干燥4至12小时,然后在真空条件下,在100至350摄氏度下,进行热扣环反应,即梯度升温反应,最后自然降温至室温,得到透明的所述聚酰亚胺薄膜。
所述芳香族二胺单体与所述二酐单体合成所述聚酰亚胺薄膜的反应通式如下:
在本实施例中,选取的是两种芳香族二胺单体与一种二酐单体反应,在其他实施例中,可选取一种芳香族二胺单体与两种二酐单体反应;在其他实施例中,也可变换所述芳香族二胺单体和所述二酐单体的加入顺序,先加入所述二酐单体,再加入所述芳香族二胺单体。因为透明聚酰亚胺薄膜需要兼顾透明和机械等综合性能,若只选取一种芳香族二胺单体和一种二酐单体,则比较难以同时兼顾透明和机械等性能。
所述硅烷偶联剂的化学键合原理如下过程所示,所述硅烷偶联剂与所述聚酰胺酸反应形成化学键,所述硅烷偶联剂水解后生成羟基,在热固化升温时,所述硅烷偶联剂上的羟基与所述玻璃基板上的羟基发生脱水反应生成化学键,使得固化后得到的所述聚酰亚胺薄膜与所述玻璃基板之间形成连接作用,进而提高该两种基材之间的附着力。
但是聚酰氨酸溶液具有一定的黏度,容易导致硅烷偶联剂分散不均匀,造成所述聚酰亚胺膜层的均匀性变差,为了改善硅烷偶联剂在聚酰胺酸溶液中分散不均的问题,本发明实施例直接在单体阶段加入硅烷偶联剂,即在溶剂中添加芳香族二胺单体(或二酐单体)之后,直接在体系中加入硅烷偶联剂,搅拌均匀后,再添加二酐单体(或芳香族二胺单体)。
本发明实施例还提供一种显示面板,所述显示面板包括衬底、薄膜晶体管阵列、以及显示层,所述显示层可为OLED发光层,也可为液晶显示层,具体可参考现有技术,这里不再赘述。所述衬底为透明的聚酰亚胺薄膜,所述聚酰亚胺薄膜采用上述方法制备。
有益效果:通过共聚的方式制备一种透明聚酰亚胺材料,在制备过程中引入了硅烷偶联剂,利用硅烷偶联剂水解后生成的羟基与玻璃基板上的羟基(在固化升温时)发生脱水反应生成化学键,进而利用这种化学键作用来增强聚酰亚胺与玻璃基板之间的附着力,从而改善因附着力差造成的两种基材分离的问题。
综上所述,虽然本发明已以优选实施例揭露如上,但上述优选实施例并非用以限制本发明,本领域的普通技术人员,在不脱离本发明的精神和范围内,均可作各种更动与润饰,因此本发明的保护范围以权利要求界定的范围为准。
Claims (10)
1.一种聚酰亚胺薄膜的制备方法,其特征在于,包括以下步骤:
步骤S10,将至少一种芳香族二胺单体溶于极性非质子有机溶剂中,并加入硅烷偶联剂,搅拌均匀以形成均相溶液,其中,所述芳香族二胺单体的结构通式如式(1)所示:H2N-R1-NH2 (1);
步骤S20,向所述均相溶液中加入至少一种二酐单体,所述二酐单体与所述芳香族二胺单体发生缩聚反应,得到聚酰胺酸溶液,其中,所述二酐单体的结构通式如式(2)所示:所述聚酰胺酸的结构通式如式(3)所示:n为正整数;
步骤S30,将所述聚酰胺酸溶液形成于玻璃基板上,进行干燥,在真空条件下,进行热扣环反应,自然降温至室温,得到所述聚酰亚胺薄膜,其中,所述聚酰亚胺的结构通式如式(4)所示:
2.根据权利要求1所述的制备方法,其特征在于,所述R1基团选自以下结构式中的一种:
3.根据权利要求1所述的制备方法,其特征在于,所述R2基团选自以下结构式中的一种:
4.根据权利要求1所述的制备方法,其特征在于,在所述步骤S20中,将所述二酐单体分3~8次加入到所述均相溶液中,所述二酐单体与所述芳香族二胺单体在室温下反应8~20小时。
5.根据权利要求1所述的制备方法,其特征在于,在所述步骤S30中,将所述聚酰胺酸溶液用300~500目的细砂布过滤,涂布到所述玻璃基板上。
6.根据权利要求5所述的制备方法,其特征在于,干燥温度为20~160摄氏度,干燥时间为4~12小时,所述热扣环反应的温度范围为100~350摄氏度。
7.根据权利要求1所述的制备方法,其特征在于,在所述步骤S10中,将两种所述芳香族二胺单体溶于极性非质子有机溶剂中,且两种所述芳香族二胺单体的摩尔比例为1:1至1:10。
8.根据权利要求7所述的制备方法,其特征在于,在所述步骤S20中,向所述均相溶液中加入一种所述二酐单体,且所述二酐单体与两种所述芳香族二胺单体总和的摩尔比为1:0.5~1:1。
9.根据权利要求1所述的制备方法,其特征在于,在所述步骤S10中,将一种芳香族二胺单体溶于所述极性非质子有机溶剂中;在所述步骤S20中,向所述均相溶液中加入两种二酐单体。
10.一种显示面板,包括衬底,其特征在于,所述衬底为如权利要求1~9任一项所述的制备方法制备的聚酰亚胺薄膜。
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