CN112334308A - 用于制造柔性器件的层合体结构以及通过使用其制造柔性器件的方法 - Google Patents
用于制造柔性器件的层合体结构以及通过使用其制造柔性器件的方法 Download PDFInfo
- Publication number
- CN112334308A CN112334308A CN201980040371.3A CN201980040371A CN112334308A CN 112334308 A CN112334308 A CN 112334308A CN 201980040371 A CN201980040371 A CN 201980040371A CN 112334308 A CN112334308 A CN 112334308A
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- Prior art keywords
- manufacturing
- flexible
- layer
- peeling force
- flexible substrate
- Prior art date
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/683—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping
- H01L21/6835—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere for supporting or gripping using temporarily an auxiliary support
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/34—Component parts, details or accessories; Auxiliary operations
- B29C41/42—Removing articles from moulds, cores or other substrates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/003—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor characterised by the choice of material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1039—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors comprising halogen-containing substituents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1042—Copolyimides derived from at least two different tetracarboxylic compounds or two different diamino compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
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Abstract
根据本发明,层合体结构包括在载体基板与柔性基板层之间的剥离力调节层,所述剥离力调节层包含聚酰亚胺,其具有比柔性基板层的折射率更高的折射率,因此可以更容易地将柔性基板从载体基板层剥离,并因此可以通过更简单的方法制造柔性器件而不损坏器件。
Description
技术领域
本申请要求于2018年11月20日提交的韩国专利申请第10-2018-0143385号和于2019年11月14日提交的韩国专利申请第10-2019-0145547号的优先权的权益,其全部公开内容通过引用并入本文。
本发明涉及具有能够促进柔性基板与载体基板的分离的剥离力调节层的层合体结构,以及使用其制造柔性器件的方法。
背景技术
显示器件市场正在将其焦点迅速改变到大尺寸、薄化且轻质的平板显示器(FPD)上。这样的平板显示器包括液晶显示器(LCD)、有机发光显示器(OLED)或电泳器件。
特别地,近年来,为了进一步扩展这样的平板显示器的应用和用途,注意力已集中在应用柔性基板的所谓的柔性显示器件上。主要考虑将柔性显示器件应用于诸如智能电话的移动器件,并且将应用领域逐渐扩展。
然而,形成和处理显示器件结构例如塑料上TFT(TFTs on plastic,TOP)的过程是制造柔性显示器件时的重要的关键过程。然而,在器件的制造过程中,在通过将柔性塑料基板直接替换现有的玻璃基板来形成器件结构时仍存在许多工艺问题。
特别地,由于包括在柔性基板中的薄膜玻璃容易因冲击而被破坏,因此显示器基板的制造过程利用在载体玻璃上的薄玻璃来进行。常规地,在载体基板例如玻璃基板上形成a-硅牺牲层等之后,在其上形成柔性基板。其后,通过玻璃基板上的器件的现有制造过程在由载体基板支撑的柔性基板上形成器件结构例如薄膜晶体管。然后,通过用激光或光照射载体基板等来破坏牺牲层以将其上形成有器件结构的柔性基板分离,最后,制造了具有柔性基板的器件,例如柔性显示器件。
然而,在现有技术的制造过程中,在激光或光的照射期间可能影响器件结构,因此可能出现缺陷,此外,需要用于激光或光照射的设备和另外的过程。因此,器件的整个制造过程变得复杂并且制造成本也大大增加。
此外,由于a-Si牺牲层等与柔性基板之间的粘合性不足,因此常常需要在牺牲层与柔性基板之间形成单独的粘合层,这可能使整个过程复杂。此外,由于需要在更苛刻的条件下进行激光或光照射,因此对其可能不利地影响器件的可靠性的担忧增加。
发明内容
技术问题
本发明要解决的问题是提供用于制造具有有助于与柔性基板层分离的剥离力调节层的柔性器件的层合体结构。
此外,本发明提供了使用所述层合体结构制造的柔性器件。
此外,本发明提供了使用所述层合体结构制造的柔性显示器。
本发明的另一个目的是提供使用所述层合体结构制造柔性器件的方法。
解决任务的手段
为了解决上述问题,本发明提供了用于制造柔性器件的层合体结构,其包括:
载体基板;
剥离力调节层,所述剥离力调节层包含聚酰亚胺并且形成在载体基板上;和
柔性基板层,所述柔性基板层形成在剥离力调节层上,
其中剥离力调节层和柔性基板层满足为0.05或更大的由以下方程式1定义的Δn值。
[方程式1]
Δn=n1-n2
其中,
n1为剥离力调节层对于550nm波长的光的TE(Transverse Electric,横向电)模式的折射率和TM(Transverse Magnetic,横向磁)模式的折射率的平均值,以及
n2为柔性基板层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值。
根据一个实施方案,剥离力调节层可以包含通过使至少一种具有式1的结构的四羧酸二酐和至少一种具有式2的结构的二胺聚合而制备的聚酰亚胺。
[式1]
[式2]
在式1和式2中,
X为包含一个或更多个脂族环或一个或更多个芳族环的四价有机基团,其中各个环结构为单环结构、各个环通过单键彼此连接、或者各个环彼此直接稠合而形成多环结构,以及
Y为包含一个或更多个芳族环或一个或更多个脂族环的二价有机基团,其中各个环结构为单环结构、各个环通过单键彼此连接、或者各个环彼此直接稠合而形成多环结构。
根据一个实施方案,X可以选自式3a至3k的四价有机基团。
式3a至3k的四价有机基团未被取代或者基团中的一个或更多个氢原子经选自具有1至10个碳原子的烷基、具有1至10个碳原子的氟烷基、具有6至12个碳原子的芳基、磺酸基和羧酸基中的取代基替代。
根据一个实施方案,Y可以选自式4a至4k的二价有机基团。
式4a至4k的二价有机基团未被取代或者基团中的一个或更多个氢原子经选自具有1至10个碳原子的烷基、具有1至10个碳原子的氟烷基、具有6至12个碳原子的芳基、磺酸基和羧酸基中的取代基替代。
根据一个实施方案,剥离力调节层可以包含含有式5的重复结构的聚酰亚胺。
[式5]
根据一个实施方案,包括式1的四羧酸二酐的二酐的总摩尔数可以小于包括式2的二胺的二胺的总摩尔数。例如,二胺的总摩尔数与二酐的总摩尔数的比率可以为100:95~99。
根据一个实施方案,柔性基板层可以包含聚酰亚胺。
根据一个实施方案,剥离力调节层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值可以为1.65至1.75。
根据一个实施方案,柔性基板层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值可以为1.55或更大且小于1.65。
根据一个实施方案,剥离力调节层的厚度可以为0.1微米至3.5微米。
此外,本发明提供了使用所述层合体结构制造柔性器件的方法。
根据一个实施方案,所述方法包括以下步骤:
在载体基板上涂覆用于制造剥离力调节层的聚酰亚胺前体组合物,然后使聚酰亚胺前体组合物在200℃至300℃的温度下固化以形成剥离力调节层;
在经固化的剥离力调节层上涂覆用于制造柔性基板的组合物并使其固化以形成柔性基板层;
在柔性基板层上形成器件;以及
将其上形成有器件的柔性基板层从其上形成有剥离力调节层的载体基板剥离,
其中剥离力调节层和柔性基板层满足为0.05或更大的由以下方程式1定义的Δn值。
[方程式1]
Δn=n1-n2
其中,
n1为剥离力调节层对于550nm波长的光的TE(横向电)模式的折射率和TM(横向磁)模式的折射率的平均值,以及
n2为柔性基板层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值。
根据一个实施方案,当将柔性基板层从涂覆有剥离力调节层的载体基板剥离时的剥离力可以为0.1N/cm或更小。
根据一个实施方案,柔性器件可以为柔性显示器件。
发明效果
根据本发明的用于制造柔性器件的层合体结构包括载体基板、柔性基板层和剥离力调节层,所述剥离力调节层设置在载体基板与柔性基板层之间并且包含具有比柔性基板层的折射率更高的折射率的聚酰亚胺,从而降低载体基板与柔性基板层之间的粘合性并且促进从载体基板剥离柔性基板层。由此,可以通过激光方法将柔性基板与载体基板分离而不损坏器件。
具体实施方式
由于可以在本发明中进行多种修改和改变,因此示出了特定的实施方案并将在具体实施方式中对其进行详细描述。然而,应理解,本发明并不旨在限于特定的实施方案,而是包括落入本发明的精神和范围内的所有修改方案、等同方案和替代方案。在以下本发明的描述中,如果确定已知功能的详细描述可能使本发明的主旨模糊,则将省略所述已知功能的详细描述。
在本说明书中,当将一个部分例如层、膜、基板等称为在另外的部分“上方”或“上”时,其不仅包括其中该部分“正好”在另外的部分上的情况,而且包括其中另一部分在其间的情况。相反地,当将一个部分例如层、膜、基板等称为在另外的部分“下方”时,其不仅包括其中该部分“正好”在另外的部分下方的情况,而且包括其中另一部分在其间的情况。
在本说明书中,除非另有说明,否则所有化合物或有机基团可以为经取代或未经取代的。在本文中,术语“经取代的”意指化合物或有机基团中包含的至少一个氢经选自以下的取代基替代:卤素原子、具有1至10个碳原子的烷基或卤代烷基、具有3至30个碳原子的环烷基、具有6至30个碳原子的芳基、羟基、具有1至10个碳原子的烷氧基、羧酸基、醛基、环氧基、氰基、硝基、氨基、磺酸基、或者其衍生物。
通常,柔性显示器通过这样来制备:在支撑基板上涂覆聚酰亚胺溶液并使其固化以形成柔性基板;在柔性基板上形成器件;然后将其上形成有器件的柔性基板与支撑基板分离。进行通过经由支撑基板将激光照射至柔性基板来剥离柔性基板的LLO(Laser LiftOff,激光举离)过程。
然而,LLO过程中使用的激光设备非常昂贵,难以维护设备并且在剥离过程期间由于高激光功率可能瞬间产生高温使得其可能影响柔性基板或器件。
本发明可以提供包括有助于将柔性基板从载体基板容易地剥离的剥离力调节层的层合体结构,由此可以在不使用激光的情况下将柔性基板从载体基板剥离。
根据本发明的用于制造柔性器件的层合体结构包括:
载体基板;
剥离力调节层,所述剥离力调节层包含聚酰亚胺并且形成在载体基板上;和
柔性基板层,所述柔性基板层形成在剥离力调节层上,
其中剥离力调节层和柔性基板层满足为0.05或更大的由以下方程式1定义的Δn值。
[方程式1]
Δn=n1-n2
其中,
n1为剥离力调节层对于550nm波长的光的TE(横向电)模式的折射率和TM(横向磁)模式的折射率的平均值,以及
n2为柔性基板层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值。
在本发明中,横向电(TE)模式的折射率和横向磁(TM)模式的折射率可以用棱镜耦合器利用550nm波长的光来测量。
根据本发明,通过在载体基板与柔性基板层之间设置包含聚酰亚胺的的剥离力调节层,可以更容易地将其上形成有器件的柔性基板从载体基板剥离。
特别地,通过使用具有比柔性基板层的折射率更高的折射率的聚酰亚胺作为剥离力调节层,可以降低与柔性基板的剥离力。例如,包含具有高折射率的聚酰亚胺的剥离力调节层可以防止用作柔性基板的上聚酰亚胺(脱粘层)扩散到下剥离力调节层中,从而实现低剥离力。在本文中,剥离力意指使柔性基板层与载体基板脱离所需的力,以及剥离力越低意指用更小的力使柔性基板层脱离。
具体地,本发明将柔性基板层的折射率与剥离力调节层的折射率之间的关系控制在其中由方程式1定义的Δn值为0.05或更大的范围内,从而通过剥离力调节层有效地调节柔性基板层的剥离力。由方程式1定义的Δn值可以为0.05或更大、0.06或更大、0.07或更大、0.075或更大、或者0.077或更大且0.1或更小、0.09或更小、0.08或更小、或者0.0785或更小。
根据一个实施方案,剥离力调节层的聚酰亚胺可以具有刚性骨架,并且具有这样的刚性骨架的分子链可以容易地堆积使得它们可以表现出高折射率。
用作剥离力调节层的聚酰亚胺可以通过例如使至少一种具有下式1的结构的四羧酸二酐和至少一种具有下式2的结构的二胺反应来制备。
[式1]
[式2]
其中,X可以为一个或更多个包含具有3至24个碳原子的脂族环或者一个或更多个具有6至30个碳原子的芳族环的四价有机基团,特别地,包含其中各个环结构为单环结构、各个环通过单键彼此连接、或者各个环彼此直接稠合而形成多环结构(即,没有任何连接基团的刚性结构)的一个或更多个脂族环或一个或更多个芳族环的四价有机基团。例如,可以提及由下式3a至3k表示的四价有机基团,但不限于此。
式3a至3k的四价有机基团中的至少一个氢原子可以经选自以下的取代基替代:具有1至10个碳原子的烷基(例如,甲基、乙基、丙基、异丙基、叔丁基、戊基、己基等)、具有1至10个碳原子的氟烷基(例如,氟甲基、全氟乙基、三氟甲基等)、具有6至12个碳原子的芳基(例如,苯基、萘基等)、磺酸基和羧酸基。
在此,式中指示的*表示键合位点。
Y为具有6至24个碳原子的单环或多环芳族二价有机基团;具有6至18个碳原子的单环或多环脂族二价有机基团;或者包含其中各个环结构为单环结构、各个环通过单键彼此连接、或者各个环彼此稠合以形成多环结构(即,没有任何连接基团的刚性结构)的一个或更多个脂族环或一个或更多个芳族环的二价有机基团。例如,可以提及由下式4a至4k表示的二价有机基团,但不限于此。
式4a至4k的二价有机基团中的至少一个氢原子可以经选自以下的取代基替代:具有1至10个碳原子的烷基(例如,甲基、乙基、丙基、异丙基、叔丁基、戊基、己基等)、具有1至10个碳原子的氟烷基(例如,氟甲基、全氟乙基、三氟甲基等)、具有6至12个碳原子的芳基(例如,苯基、萘基等)、磺酸基和羧酸基。
根据一个实施方案,相对于具有式1的结构的酸二酐的总摩尔量,式2的二胺的总摩尔量可以以过量聚合。例如,二胺与酸二酐的总摩尔比可以为100:95~99,最优选地100:96~97。当二胺与酸二酐的摩尔比为合适的比率时,可以抑制聚酰胺酸溶液的凝胶化以形成具有均匀表面的涂层,并且易于将涂层厚度均匀地调节至一定厚度。
根据一个实施方案,包含在剥离力调节层中的聚酰亚胺可以包含下式5的重复结构。
[式5]
根据一个实施方案,剥离力调节层对于550nm波长的光的TE模式的折射率可以为1.75或更大、1.78或更大、1.79或更大或者1.80或更大且1.85或更小、1.84或更小、1.83或更小、1.82或更小或者1.81或更小。TM模式的折射率可以为1.49或更大、1.52或更大或者1.55或更大且1.65或更小、1.63或更小、1.60或更小或者1.59或更小。TE模式的折射率和TM模式的折射率的平均值可以为1.65或更大、1.66或更大、1.68或更大或者1.69或更大且1.75或更小、1.72或更小或者1.70或更小。
根据本发明,柔性器件可以通过包括以下步骤的方法来制造:
在载体基板上涂覆用于制造剥离力调节层的聚酰亚胺前体组合物,然后使聚酰亚胺前体组合物在200℃至300℃的温度下固化以形成剥离力调节层;
在剥离力调节层上涂覆用于制造柔性基板的组合物并使其固化以形成柔性基板层;
在柔性基板层上形成器件;以及
将其上形成有器件的柔性基板层从其上形成有剥离力调节层的载体基板剥离。
根据一个实施方案,剥离力调节层可以以0.1微米或更大、0.5微米或更大或者1微米或更大且3.5微米或更小、3微米或更小或者2微米或更小的厚度涂覆在载体基板上。
根据一个实施方案,在将柔性基板层从其上形成有剥离力调节层的载体基板剥离时,剥离力可以为0.1N/cm或更小、0.07N/cm或更小、0.05N/cm或更小且0.01N/cm或更大、或者0.02N/cm或更大。
当剥离强度高于0.1N/cm时,柔性基板层的剥离可能不容易,或者在剥离过程期间可能发生对形成在柔性基板上的器件的损坏。因此,其可能难以作为剥离力调节层应用。
剥离力调节层和柔性基板层可以通过物理刺激来分离,物理刺激意指仅用物理力剥离而不引起化学变化。
通过在载体基板与用作柔性显示器件的基板的柔性基板之间设置根据本发明的包含聚酰亚胺树脂的剥离力调节层,即使省略激光或光照射过程并且仅施加物理刺激,也可以容易地将柔性基板与剥离力调节层分离,因此可以容易地制造具有柔性基板的器件例如柔性显示器件。这是因为使用具有高折射率的聚酰亚胺作为剥离力调节层,从而防止设置在剥离力调节层上的柔性基板层的聚合物例如聚酰亚胺扩散到剥离力调节层中以降低剥离力。
作为柔性基板,可以没有特别限制地包含适用于柔性器件的基板的任何已知的聚合物。其具体实例可以包括选自以下中的至少一者:聚醚砜、聚萘二甲酸乙二醇酯、聚对苯二甲酸乙二醇酯、聚碳酸酯、聚酰亚胺、聚醚酰亚胺、聚酰胺酰亚胺、聚酯、聚醚酰胺酰亚胺、聚酯酰胺酰亚胺和聚芳酯,更优选地基于聚酰亚胺的树脂,并且聚酰亚胺的类型没有特别限制。
根据一个实施方案,包含在柔性基板层中的聚合物树脂的TE模式的折射率可以为1.65或更大、1.67或更大且1.70或更小、1.69或更小、1.68或更小或者1.672或更小。TM模式的折射率可以为1.50或更大、1.54或更大或者1.55或更大且1.60或更小、1.58或更小或者1.57或更小。TE模式的折射率和TM模式的折射率的平均值可以为1.55或更大、1.58或更大或者1.60或更大且小于1.65或者1.64或更小、1.63或更小或者1.62或更小。
用于制备用于脱粘层和柔性基板层的聚酰亚胺的酸二酐和二胺化合物的聚合反应可以根据聚酰亚胺或其前体的常规聚合方法例如溶液聚合来进行。
反应可以在无水条件下进行,并且在聚合反应期间的反应温度可以为-75℃至50℃,优选地0℃至40℃。反应可以通过在将二胺化合物溶解在有机溶剂中的同时添加酸二酐来进行。
此外,特别地,可以用于聚合反应的有机溶剂可以选自酮,例如γ-丁内酯、1,3-二甲基-咪唑烷酮、甲基乙基酮、环己酮、环戊酮和4-羟基-4-甲基-2-戊酮;芳族烃,例如甲苯、二甲苯和四甲基苯;二醇醚(溶纤剂),例如乙二醇单乙醚、乙二醇单甲醚、乙二醇单丁醚、二乙二醇单乙醚、二乙二醇单甲醚、二乙二醇单丁醚、丙二醇单甲醚、丙二醇单乙醚、二丙二醇二乙醚和三乙二醇单乙醚;乙酸乙酯;乙酸丁酯;乙二醇单乙醚乙酸酯;乙二醇单丁醚乙酸酯;二乙二醇单乙醚乙酸酯;二丙二醇单甲醚乙酸酯;乙醇;丙醇;乙二醇;丙二醇;卡必醇;二甲基乙酰胺(DMAc);N,N-二乙基乙酰胺(DEAc);二甲基甲酰胺(DMF);二乙基甲酰胺(DEF);N-甲基吡咯烷酮(NMP);N-乙基吡咯烷酮(NEP);N-乙烯基吡咯烷酮;1,3-二甲基-2-咪唑烷酮;N,N-二甲基甲氧基乙酰胺;二甲基亚砜;吡啶;二甲基砜;六甲基磷酰胺;四甲基脲;N-甲基己内酰胺;四氢呋喃;间二烷;对二烷;1,2-二甲氧基乙烷;双(2-甲氧基乙基)醚;1,2-双(2-甲氧基乙氧基)乙烷;双[2-(2-甲氧基乙氧基)]醚;及其混合物。
此外,在合成聚酰胺酸或聚酰亚胺的情况下,可以进一步添加其中分子的末端与二羧酸酐或单胺反应以使聚酰亚胺的末端封端的封端剂而使过量的多氨基或酸酐基失活。
使用所制备的聚酰亚胺前体组合物制备聚酰亚胺的方法包括将聚酰亚胺前体组合物施加至基板的一个表面并使其酰亚胺化和固化。
具体地,聚酰亚胺前体组合物可以为溶解在有机溶剂中的溶液的形式,在具有这种形式的情况下,例如,当在有机溶剂中合成聚酰亚胺前体时,聚酰亚胺前体组合物可以是聚合之后所获得的聚酰亚胺前体溶液其本身或者通过另外添加相同的溶液而获得的溶液,或者可以通过将聚合之后获得的聚酰亚胺前体溶液用另外的溶剂稀释而获得。
考虑到成膜过程中的可加工性例如涂覆特性,聚酰亚胺前体组合物可以以使得聚酰亚胺前体组合物具有合适的粘度的量包含固体,并且基于聚酰亚胺前体组合物的总重量,固体含量可以为5重量%至20重量%。或者,可以优选将聚酰亚胺前体组合物调节为具有400cP至50,000cP的粘度。聚酰亚胺前体组合物的粘度可以小于400cP。当聚酰亚胺前体组合物的粘度大于50,000cP时,在使用聚酰亚胺前体组合物制造显示器基板期间,流动性可能降低,这可能在制造过程中引起问题,例如不均匀涂覆。
作为载体基板,可以没有任何特别限制地使用玻璃基板、金属基板、塑料基板等。其中,可以优选玻璃基板,其在聚酰亚胺前体的酰亚胺化和固化过程期间热稳定性和化学稳定性优异,并且即使在不用另外的脱模剂进行任何处理的情况下也可以容易地分离,同时不损坏固化之后形成的聚酰亚胺膜。
施加或涂覆过程可以根据常规施加方法来进行。具体地,可以使用旋涂法、棒涂法、辊涂法、气刀法、凹版印刷法、反向辊法、舐涂辊法、刮刀法、喷雾法、浸渍法、刷涂法等。
其中,更优选通过允许连续过程并且能够提高聚酰亚胺树脂的酰亚胺化率的流延法来进行。
此外,可以以使得最终制备的聚酰亚胺膜具有适用于剥离力调节层或显示器基板的厚度的厚度范围将聚酰亚胺前体溶液施加在基板上。例如,柔性基板层的厚度可以为至少5微米、至少10微米、至少12微米或至少15微米且至多30微米、或至多20微米。
在施加聚酰亚胺前体组合物之后,可以在固化过程之前进一步任选地进行用于除去聚酰亚胺前体组合物中剩余的溶剂的干燥过程。
干燥过程可以根据常规方法来进行。具体地,干燥过程可以在140℃或更低或者80℃至140℃的温度下进行。如果干燥温度低于80℃,则干燥过程变得更长。如果干燥温度超过140℃,则酰亚胺化可能快速地进行,使得难以形成具有均匀厚度的聚酰亚胺膜。
剥离力调节层的固化过程可以通过在200℃至300℃的温度下进行热处理来进行。
随后,包含在柔性基板层中的聚酰亚胺的固化过程可以通过在300℃至400℃的温度下的热处理来进行。固化过程可以在上述温度范围内以多步加热过程来进行。此外,固化过程中的固化时间没有特别限制,例如为3分钟至30分钟。
此外,在形成剥离力调节层时的固化过程之后,可以进一步任选地进行后续热处理过程以提高聚酰亚胺膜中的聚酰亚胺树脂的酰亚胺化率以形成具有上述物理特性的聚酰亚胺膜。
后续热处理过程优选在200℃或更高、或者200℃至450℃下进行1分钟至30分钟。此外,后续热处理过程可以进行一次或者可以以多个阶段进行两次或更多次。具体地,其可以以包括在200℃至220℃下的第一热处理、在300℃至380℃下的第二热处理、和在400℃至450℃下的第三热处理的三步进行。
包含在柔性基板层中的聚酰亚胺的玻璃化转变温度可以为约330℃或更高。由于其具有这样的优异耐热性,因此包含聚酰亚胺的膜针对在器件的制造过程期间施加的高温热可以保持优异的耐热性和机械特性。
根据本发明的层合体结构可以特别有用地制造电子器件(例如,OLED或LCD、电子纸、太阳能电池)中的柔性器件。
发明实施方式
在下文中,将详细地描述本发明的实施方案使得本领域技术人员可以容易地实施本发明。然而,本发明可以以许多不同的形式体现并且不应被解释为限于本文所阐述的实施方案。
<实施例1>
在氮气氛下将0.095mol PDA(对苯二胺)溶解在100g DEAc(N,N-二乙基乙酰胺)中,然后添加0.0917mol PMDA(均苯四酸二酐)和80g DEAc作为另外的溶剂并反应48小时以制备聚酰胺酸溶液。将聚酰胺酸溶液稀释至合适的浓度,以1微米的厚度涂覆在玻璃基板上,并在250℃下固化以制备剥离力调节层。
为了形成柔性基板层,将0.0666mol TFMB(2,2’-双(三氟甲基)-4,4’-二氨基联苯)溶解在70g DEAc中,然后添加0.033mol PMDA和0.033mol BPDA以及150g DEAc作为另外的溶剂并反应48小时以制备聚酰胺酸溶液。将聚酰胺酸溶液(TFMB-PMDA/BPDA)以15微米的厚度涂覆在剥离力调节层上,并在300℃下固化以制备具有所形成的柔性基板层的层合体结构。
<比较例1>
在氮气氛下将0.0666mol TFMB(2,2’-双(三氟甲基)-4,4’-二氨基联苯)溶解在70g DEAc中,然后添加0.033mol PMDA和0.033mol BPDA以及150g DEAc作为另外的溶剂并反应48小时以制备聚酰胺酸溶液。
将聚酰胺酸溶液以1微米的厚度涂覆在玻璃基板上,并在250℃下固化以制备剥离力调节层。然后,将相同的聚酰胺酸溶液以15微米的厚度涂覆在剥离力调节层上,并在300℃下固化以制备具有所形成的柔性基板层的层合体结构。
<实施例2至4>
以与如实施例1中相同的方式制备层合体结构,不同之处在于如表1所示调节酸二酐与二胺的摩尔比。
<实验例1>
<折射率的测量>
使用Metricon 2010M棱镜耦合器测量剥离力调节层和柔性基板层中的聚酰亚胺对于550nm波长的光的TE(横向电)模式和TM(横向磁)模式的折射率。
基于所测量的折射率计算方程式1的Δn值并将其示于下表1中。
[方程式1]
Δn=n1-n2
n1为剥离力调节层对于550nm波长的光的TE(横向电)模式的折射率和TM(横向磁)模式的折射率的平均值,以及
n2为柔性基板层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值。
<剥离力的测量>
将层合体结构切割成宽度为10mm且长度为100mm的矩形形状并通过使用质构分析仪(TA,XT plus,Stable microsystems)测量在保持柔性基板的端部的同时以50mm/分钟剥离切割的柔性基板的力。
折射率和剥离力的测量结果示于表1中。
[表1]
根据以上结果,在其中由剥离力调节层和柔性基板的折射率计算的Δn值满足0.05或更大的实施例1和2的情况下,剥离力降低至比较例1的剥离力的1/10的水平。此外,在实施例3和4中,获得远低于比较例1的剥离力的0.1N/cm或更小的剥离力。
据此,可以看出在使用根据本发明的剥离力调节层的情况下,实际过程中可以更容易地制造柔性器件。
然而,在实施例3中,剥离力调节层的表面有些不均匀,因为用于形成剥离力调节层的溶液发生凝胶化,以及在实施例4中,用于形成剥离力调节层的溶液的粘度低,使得难以适当地形成剥离力调节层的厚度。因此,例如,当使用PDA和PMDA制造剥离力调节层时,最优选的摩尔比可以为100:96~97。
虽然已经参照本发明的具体实施方案特别示出和描述了本发明,但是对于本领域技术人员来说明显的是,该具体描述仅仅是优选的实施方案并且本发明的范围不限于此。因此,本发明的范围旨在由本文所附的权利要求书及其等同方案来限定。
Claims (15)
1.一种用于制造柔性器件的层合体结构,包括:
载体基板;
剥离力调节层,所述剥离力调节层包含聚酰亚胺并且形成在所述载体基板上;和
柔性基板层,所述柔性基板层形成在所述剥离力调节层上,
其中所述剥离力调节层和所述柔性基板层满足为0.05或更大的由以下方程式1定义的Δn值:
[方程式1]
Δn=n1-n2
其中,
n1为所述剥离力调节层对于550nm波长的光的TE(横向电)模式的折射率和TM(横向磁)模式的折射率的平均值,以及
n2为所述柔性基板层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值。
6.根据权利要求2所述的用于制造柔性器件的层合体结构,其中包含式1的所述四羧酸二酐的二酐的总摩尔数小于包含式2的所述二胺的二胺的总摩尔数。
7.根据权利要求6所述的用于制造柔性器件的层合体结构,其中所述二胺的总摩尔数与所述二酐的总摩尔数的比率为100:95~99。
8.根据权利要求1所述的用于制造柔性器件的层合体结构,其中所述柔性基板层包含聚酰亚胺。
9.根据权利要求1所述的用于制造柔性器件的层合体结构,其中所述剥离力调节层对于550nm波长的光的所述TE模式的折射率和所述TM模式的折射率的平均值为1.65至1.75。
10.根据权利要求1所述的用于制造柔性器件的层合体结构,其中所述柔性基板层对于550nm波长的光的所述TE模式的折射率和所述TM模式的折射率的平均值为1.55或更大且小于1.65。
11.根据权利要求1所述的用于制造柔性器件的层合体结构,其中所述剥离力调节层的厚度为0.1微米至3.5微米。
12.一种用于制造柔性器件的方法,使用根据权利要求1至11中任一项所述的层合体结构。
13.一种用于制造柔性器件的方法,包括以下步骤:
在载体基板上涂覆用于制造剥离力调节层的聚酰亚胺前体组合物,然后使所述聚酰亚胺前体组合物在200℃至300℃的温度下固化以形成剥离力调节层;
在所述剥离力调节层上涂覆用于制造柔性基板的组合物并使其固化以形成柔性基板层;
在所述柔性基板层上形成器件;以及
将其上形成有所述器件的所述柔性基板从其上形成有所述剥离力调节层的所述载体基板剥离,
其中所述剥离力调节层和所述柔性基板层满足为0.05或更大的由以下方程式1定义的Δn值:
[方程式1]
Δn=n1-n2
其中,
n1为所述剥离力调节层对于550nm波长的光的TE(横向电)模式的折射率和TM(横向磁)模式的折射率的平均值,以及
n2为所述柔性基板层对于550nm波长的光的TE模式的折射率和TM模式的折射率的平均值。
14.根据权利要求13所述的用于制造柔性器件的方法,其中当将所述柔性基板层从涂覆有所述剥离力调节层的所述载体基板剥离时的剥离力为0.1N/cm或更小。
15.根据权利要求13所述的用于制造柔性器件的方法,其中所述柔性器件为柔性显示器件。
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