CN107033798B - 表面保护膜、制造方法和衬底加工层叠体 - Google Patents
表面保护膜、制造方法和衬底加工层叠体 Download PDFInfo
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- CN107033798B CN107033798B CN201710063886.8A CN201710063886A CN107033798B CN 107033798 B CN107033798 B CN 107033798B CN 201710063886 A CN201710063886 A CN 201710063886A CN 107033798 B CN107033798 B CN 107033798B
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- -1 silylphenylene-siloxane skeleton Chemical group 0.000 claims abstract description 77
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- ILLOBGFGKYTZRO-UHFFFAOYSA-N tris(2-ethylhexyl) phosphite Chemical compound CCCCC(CC)COP(OCC(CC)CCCC)OCC(CC)CCCC ILLOBGFGKYTZRO-UHFFFAOYSA-N 0.000 description 1
- OOZBTDPWFHJVEK-UHFFFAOYSA-N tris(2-nonylphenyl) phosphate Chemical compound CCCCCCCCCC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)CCCCCCCCC)OC1=CC=CC=C1CCCCCCCCC OOZBTDPWFHJVEK-UHFFFAOYSA-N 0.000 description 1
- FEVFLQDDNUQKRY-UHFFFAOYSA-N tris(4-methylphenyl) phosphite Chemical compound C1=CC(C)=CC=C1OP(OC=1C=CC(C)=CC=1)OC1=CC=C(C)C=C1 FEVFLQDDNUQKRY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C08J7/08—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/14—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/06—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
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- 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
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- C08G2261/12—Copolymers
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Abstract
本发明为表面保护膜、制造方法和衬底加工层叠体。能够将包括基膜和其上的树脂膜的表面保护膜与具有电路形成表面的衬底接合并且在加工后与其分离。该树脂膜由树脂组合物形成,该树脂组合物包括(A)含有硅亚苯基‑硅氧烷骨架的树脂、(B)能够与该树脂中的环氧基反应以形成交联结构的化合物、(C)固化催化剂、和(D)脱模剂。
Description
相关申请的交叉引用
本非临时申请在35U.S.C.§119(a)下要求于2016年2月4日在日本提交的专利申请No.2016-019725的优先权,由此通过引用将其全部内容并入本文。
技术领域
本发明涉及可在衬底的加工过程中使用的表面保护性材料。与具有待保护的表面的衬底的处理相关联,该处理包括衬底中通孔或贯通电极的形成和衬底的精密加工(例如,电路形成),本发明涉及表面保护膜,将该表面保护膜临时地接合于衬底表面以保护表面免受缺陷、冲击、污渍等。其也涉及衬底加工层叠体和制备表面保护膜的方法。
背景技术
目前的电子技术在探究具有多个竖直堆叠的半导体部件的堆叠结构。与该堆叠结构相关联,制造半导体芯片的方法包括如下步骤:将高纯度硅单晶锭切成晶片;在该晶片的前表面上形成所需的电路图案以形成集成电路;采用研磨机对该晶片的背表面进行研磨至约25-200μm的晶片厚度;贯通晶片打孔;在其中形成电极,称为硅通孔(TSV);和在竖直方向上将TSV电极连接以由此增加集成度。
在采用TSV之前,在硅衬底上形成电路的步骤中,必须认真检查衬底的背表面是否被损伤或污染,原因在于电路只在前表面上。在前表面和背表面上都形成并且连接电路的TSV结构中,有必要在加工一表面时保护另一表面。要求在该步骤中使用的保护部件具有耐热性、耐压性和耐化学性。另外要求在加工结束时能够容易地将该保护部件除去。
在该应用中,接合力和耐压性是关键的。具体地,必须使保护部件接合于晶片或衬底而没有留下间隙,并且具有充分的接合力和耐压性以承受随后的步骤。在加工结束时,能够将保护部件顺利地从晶片或衬底剥离而没有在衬底表面上留下任何树脂残渣、树脂组分或添加剂组分。
目前为止,致力于用于保护晶片表面的表面保护膜和树脂组合物。例如,专利文献1公开了可借助UV剥离的旨在用于晶片背面研磨的表面保护膜。一旦使该膜接合于晶片的前表面,则在保护前表面(例如,电路)的同时可对背表面进行研磨。为了去除而照射UV,这意味着剥离步骤繁杂,或者昂贵的UV照射设备是必需的。增加的步骤费用是不利的。专利文献2公开了没有将UV用于去除的旨在用于晶片背面研磨的表面保护性带材。在背表面研磨过程中使该带材适应于前表面保护。该带材具有强接合力使得在背表面研磨过程中即使在重冲击下也不会使该带材分离。反过来这意味着该带材难以剥离,暗示将该带材从中剥离时能够使薄晶片断裂的危险性。由于该带材旨在用于背表面研磨,因此没有预期使用水以外的溶剂。如果使用溶剂,则能够使该带材中的粘合剂组分溶解或改变。存在将该带材不经意地或者困难地从晶片表面剥离的可能性。对于背表面研磨以外的应用,在专利文献3中公开了蚀刻过程中使用的保护膜。该保护膜在蚀刻过程中具有耐化学性。该膜包括薄的压敏粘合剂层,其难以填埋衬底表面上的凹凸(例如,电路和通孔)。
引用列表
专利文献1:JP-A 2014-017336
专利文献2:JP-A 2013-199623
专利文献3:JP-A H10-284444
发明内容
本发明的目的是提供表面保护膜,其可接合于衬底,对在电路形成或者另外衬底的加工中采用的化学品、热和压力具有耐受性,并且在加工结束时可从衬底剥离而无需UV照射等并且没有留下残渣;使用其的衬底加工层叠体;及其制备方法。
本发明人已发现包括具有硅亚苯基-硅氧烷骨架的树脂的固化性树脂组合物具有高耐热性、高耐压性、高耐化学性和适度的接合力,并且该树脂组合物形成表面保护膜,该表面保护膜可接合于衬底并且在衬底的处理和加工过程中最适宜。
因此,一方面,本发明提供表面保护膜,其包括基膜和在其上形成的树脂膜,所述树脂膜由包括组分(A)-(D)的树脂组合物形成:
(A)由式(1)表示并且具有10,000-100,000的重均分子量的含有硅亚苯基-硅氧烷骨架的树脂,
(B)能够与该含有硅亚苯基-硅氧烷骨架的树脂中的环氧基反应以形成交联结构的化合物,
(C)固化催化剂,和
(D)脱模剂,其选自由聚乙烯、有机硅化合物、氟化合物、脂肪酸和脂肪酸酯组成的组,其量为0.5-20重量份,相对于100重量份的组分(A)。
其中R1和R6各自独立地为C1-C20一价烃基或烷氧基;a、b、c、和d表示对应的重复单元的组成比,为满足:0<a<1,0<b<1,0≤c<1,0<d<1,0.35≤a+c≤0.65,0.35≤b+d≤0.65,和a+b+c+d=1的正数,g为0-300的整数;X为具有式(2)的二价有机基团:
其中E为选自下述的二价有机基团:
s为0或1,R7和R8各自独立地为C1-C20一价烃基或烷氧基,t和u各自独立地为0-2的整数;并且Y为具有式(3)的二价硅氧烷链:
其中R9-R14各自独立地为C1-C20一价烃基或烷氧基,并且j为0-300的整数。
优选地,在式(1)中,a、b、c和d满足a+c=0.5并且b+d=0.5。
在优选的实施方案中,形成树脂膜的组合物还包括(E)阻燃剂、(F)抗氧化剂、和(G)填料中的至少一种组分。
典型地,该基膜由聚酯、聚酰亚胺、聚酰胺、聚酰胺-酰亚胺、聚醚酰亚胺、三乙酸纤维素、聚醚砜或聚苯硫醚形成。
在另一方面中,本发明提供衬底加工层叠体,其包括衬底和设置在该衬底的至少一个表面上的表面保护膜(如上所定义)。
在另一方面中,本发明提供表面保护膜的制备方法,该表面保护膜包括基膜和其上形成的树脂膜,该方法包括:将表面保护性树脂组合物施涂到该基膜上的步骤、和将该组合物加热固化为该树脂膜的步骤,该树脂组合物包括以上定义的组分(A)-(D)。
在又一方面中,本发明提供保护具有电路形成表面的衬底的方法,包括:使以上定义的表面保护膜附接于该衬底的电路形成表面的步骤,和将该树脂膜加热固化以使该表面保护膜与该衬底接合。
发明的有利效果
由于该表面保护膜由包括含有硅烷(甲硅烷基苯)骨架的树脂和脱模剂的树脂组合物形成,因此将接合力调节到适度的水平使得与衬底接合的膜可在衬底的加工过程中难以被剥离,但在加工结束时顺利地被剥离。该膜最适合于与衬底的临时接合。
由于该树脂含有硅亚苯基骨架并因此具有高强度,所以在剥离时不会使表面保护膜破裂。能够在没有将任何树脂和添加剂残渣留在衬底上的情况下将该膜剥离。由于该树脂为热固性树脂,因此该膜具有耐热性和耐压性并且在衬底的加工过程中避免任何麻烦。此外,由于该表面保护膜中的脱模剂发挥缓和由固化树脂的热膨胀诱发的内部应力的功能,因此该膜即使在高温下也不可能剥离。
一旦用该表面保护膜保护该衬底,则受保护的衬底表面在衬底的加工和处理过程中长期不会被损伤或沾污。可预期失效率的减小。由于只涉及直接涂布和加热固化步骤,因此制备表面保护膜的方法容易。
具体实施方式
标记(Cn-Cm)意指每个基团含有n至m个碳原子的基团。化学式中,Me表示甲基,并且Ph表示苯基。
表面保护膜
本发明的一个实施方案为表面保护膜,其包括基膜和在其上形成的树脂膜。
该树脂膜由树脂组合物形成,该树脂组合物包括:(A)含有硅亚苯基-硅氧烷骨架的树脂,(B)能够与该树脂中的环氧基反应以形成交联结构的化合物,(C)固化催化剂,和(D)脱模剂。
(A)含有硅亚苯基-硅氧烷骨架的树脂
组分(A)为由式(1)表示的含有硅亚苯基-硅氧烷骨架的树脂。
式(1)中,R1-R6可以相同或不同,各自独立地为C1-C20一价烃基或烷氧基。该一价烃基包括直链、支化或环状烷基、烯基和炔基,但并不限于此。优选地,R1-R6为C1-C12一价烃基或烷氧基,更优选为C1-C10一价烃基或烷氧基,甚至更优选为C1-C6一价烃基或烷氧基。
以下给出R1-R6的优选的实例。
-CH3,-CH2-CH3,-(CH2)4-CH3,-(CH2)6-CH3,-(CH2)8-CH3,
-(CH2)10-CH3,-(CH2)15-CH3,-(CH2)19-CH3,-CH=CH-CH3,
-C≡C-CH3,-CH=CH-CH=CH-CH3,-CH=CH-C≡C-CH3,-CH(CH3)-CH3,
-C(CH3)(CH3)-CH3,-CH2-CH(CH3)-CH3,-CH2-CH(CH3)-CH(CH3)-CH3,
-CH2-CH(CH2CH2CH3)-CH3,-CH2-C(CH2CH2CH3)(CH2CH2CH3)-CH3,
-CH2-C(CH2CH(CH3)CH3)(CH2CH2CH3)-CH3,
-CH2-C(CH2CH(CH3)CH3)(CH2C(CH3)(CH3)CH3)-CH3,
-OCH3,-OCH2CH3,-OCH(CH3)CH3,-O(CH2)3CH3,-OC(CH3)2C≡CH
下标a、b、c和d表示对应的重复单元的组成比,为满足以下条件的正数:0<a<1,0<b<1,0≤c<1,0<d<1,0.35≤a+c≤0.65,0.35≤b+d≤0.65和a+b+c+d=1,优选地a+b>c。如果a和c之和或者b和d之和在该范围之外,聚合物具有低分子量。更优选地,a、b、c和d满足a+c=0.5并且b+d=0.5。下标g为0-300的整数。
式(1)的树脂中,基于全部重复单元,优选以40-80重量%、更优选地50-75重量%、甚至更优选地60-70重量%的量含有硅氧烷单元。如果硅氧烷单元含量低于该范围,则剥离可能变沉滞。如果硅氧烷单元含量高于该范围,则剥离力可能变低,表明在加工过程中可能剥离。在式(1)的树脂中,基于全部重复单元,优选以2-15重量%、更优选地3-12重量%、甚至更优选地4-8重量%的量含有硅亚苯基单元。如果硅亚苯基单元含量高于该范围,则树脂变得太硬使得剥离时树脂可能破裂,在衬底表面上留下树脂残渣。如果硅亚苯基单元含量低于该范围,则该树脂缺少强度使得该树脂在剥离时可能破裂,剥离后留下树脂残渣。
式(1)中,X为具有式(2)的二价有机基团。
E为选自下述的二价有机基团。
下标s为0或1,R7和R8各自独立地为C1-C20一价烃基或烷氧基,t和u各自独立地为0-2的整数。
式(2)中,R7和R8各自独立地为C1-C20一价烃基或烷氧基。该一价烃基包括直链、支化或环状烷基、烯基和炔基,但并不限于此。优选地,R7和R8为C1-C12一价烃基或烷氧基,更优选为C1-C10一价烃基或烷氧基,甚至更优选为C1-C6一价烃基或烷氧基。
以下给出R7和R8的优选实例。
-CH3,-CH2-CH3,-(CH2)4-CH3,-(CH2)6-CH3,-(CH2)8-CH3,
-(CH2)10-CH3,-(CH2)15-CH3,-(CH2)19-CH3,-CH=CH-CH3,-C≡C-CH3,
-CH=CH-CH=CH-CH3,-CH=CH-C≡C-CH3,-CH(CH3)-CH3,-C(CH3)(CH3)-CH3,
-CH2-CH(CH3)-CH3,-CH2-CH(CH3)-CH(CH3)-CH3,-CH2-CH(CH2CH2CH3)-CH3,
-CH2-C(CH2CH2CH3)(CH2CH2CH3)-CH3,
-CH2-C(CH2CH(CH3)CH3)(CH2CH2CH3)-CH3,
-CH2-C(CH2CH(CH3)CH3)(CH2C(CH3)(CH3)CH3)-CH3,
-OCH3,-OCH2CH3,-OCH(CH3)CH3,-O(CH2)3CH3,-OC(CH3)2C≡CH,
式(2)中,s为0或1,t和u各自独立地为0-2的整数。
式(1)中,Y为具有式(3)的二价硅氧烷链。
式(3)中,R9-R14可以相同或不同,各自独立地为C1-C20一价烃基或烷氧基。一价烃基包括直链、支化或环状烷基、烯基、炔基和芳基,但并不限于此。也包括其中至少一个氢原子被芳基取代的烷基、烯基和炔基,和其中至少一个氢原子被烷基、烯基或炔基取代的芳基,条件是被取代了的基团中碳原子的总数为20以下。
优选地,R9-R14为C1-C12一价烃基,更优选为C1-C10一价烃基,甚至更优选为C1-C6烷基或苯基。
以下给出R9-R14的优选实例。
-CH3,-CH2-CH3,-(CH2)4-CH3,-(CH2)6-CH3,-(CH2)8-CH3,
-(CH2)10-CH3,-(CH2)15-CH3,-(CH2)19-CH3,-CH=CH-CH3,-C≡C-CH3,
-CH=CH-CH=CH-CH3,-CH=CH-C≡C-CH3,-CH(CH3)-CH3,-C(CH3)(CH3)-CH3,
-CH2-CH(CH3)-CH3,-CH2-CH(CH3)-CH(CH3)-CH3,-CH2-CH(CH2CH2CH3)-CH3,
-CH2-C(CH2CH2CH3)(CH2CH2CH3)-CH3,
-CH2-C(CH2CH(CH3)CH3)(CH2CH2CH3)-CH3,
-CH2-C(CH2CH(CH3)CH3)(CH2C(CH3)(CH3)CH3)-CH3,
-OCH3,-OCH2CH3,-OCH(CH3)CH3,-O(CH2)3CH3,-OC(CH3)2C≡CH,苯基。
式(3)中,j为0-300的整数、优选地0-200的整数、更优选地30-150的整数、甚至更优选地50-100的整数。如果j大于300,使接合力显著地减小,有可能在加工过程中膜从衬底表面剥离。
以下给出具有式(3)的基团的实例,但并不限于此。
以下给出具有式(1)的树脂的实例,但并不限于此。
树脂(A)应具有10,000-100,000、优选地25,000-60,000的重均分子量(Mw)。Mw小于10,000的树脂有时可能不是固体,不足以作为成膜材料,而Mw超过100,000的树脂太粘稠以致无法处理。本说明书中,通过使用四氢呋喃溶剂的凝胶渗透色谱(GPC)相对于聚苯乙烯标样测量Mw。
树脂(A)中,各个单元可以无规排列或嵌段排列(以形成无规共聚物或嵌段共聚物)。
可采用下述的方法使用具有式(4)的硅亚苯基化合物和选自具有式(5)-(7)的化合物中的化合物来制备树脂(A)。
其中R1-R14、E、g、s、t、u和j如上所定义。
树脂(A)可以通过反应物的氢化硅烷化而合成。一个工序中,将全部反应物供给到实施反应的反应器中。在另一个工序中,预先使一些反应物反应,然后供给剩余的反应物并使其反应。在又一个工序中,使反应物逐步地反应。在任何情况下,反应的顺序是任意的。
在催化剂的存在下进行聚合反应。可以使用任何已知促进氢化硅烷化的催化剂。例如,可以使用钯络合物、铑络合物和铂络合物,但催化剂并不限于此。相对于Si-H键,优选以约0.01-10.0mol%的量添加催化剂。催化剂的量较少时,反应可能缓慢或者在较小的程度上进行。较大量的催化剂可能引起脱氢反应,其干扰加成反应的进行。
聚合反应可在溶剂中进行,该溶剂选自不干扰氢化硅烷化的有机溶剂。适合的溶剂包括辛烷、甲苯、四氢呋喃和二噁烷,但并不限于此。优选以给予10-70重量%的溶质浓度的量使用该溶剂。如果溶剂的量大于该范围,则反应体系太稀薄使得反应的进行可能缓慢。如果溶剂的量小于该范围,则反应体系太粘稠使得在中途抑制有效的搅拌。
典型地,该反应在40-150℃、优选地60-120℃、更优选地70-100℃的温度下进行。在该范围外时,在较高温度下可能发生副反应例如分解,而在较低温度下的反应进行缓慢。反应时间典型地为0.5-60小时,优选为3-24小时,更优选为5-12小时。
(B)交联化合物
组分(B)为能够与含有硅亚苯基-硅氧烷骨架的树脂(A)中的环氧基反应以形成交联结构的化合物。其优选为每分子含有至少两个酚羟基的化合物,但并不限于此。每分子的酚羟基的数目优选为2-约10。每分子只含有一个酚羟基的化合物无法交联,使得没有使树脂固化。每分子含有大于10个酚羟基的化合物引起显著的固化收缩并且不实用。只要酚羟基的数目在该范围内,则对该化合物的结构并无特别限制。以下给出优选的例示性化合物。
相对于100重量份的组分(A),优选以5-50重量份、更优选以8-20重量份的量使用组分(B)。只要组分(B)的量在该范围内,则组分(B)与组分(A)充分地反应使得固化物变得更为强韧。
(C)固化催化剂
组分(C)为固化催化剂,其选自用于环氧基的开环的各种催化剂。适合的固化催化剂包括,但并不限于,咪唑化合物例如咪唑、2-甲基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、1,2-二甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-苄基-2-甲基咪唑、1-氰基乙基-2-甲基咪唑、1-氰基乙基-2-十一烷基咪唑、1-氰基乙基-2-乙基-4-甲基咪唑、1-氰基乙基-2-苯基咪唑、2-苯基-4,5-二羟基甲基咪唑、和2-苯基-4-甲基-5-羟基甲基咪唑;和1,8-二氮杂双环[5.4.0]-十一碳烯-7、三(二甲基氨基甲基)苯酚、三苯基膦、和四苯基鏻四苯基硼酸盐。
相对于100重量份的组分(A),优选以0.01-30重量份、更优选以1-5重量份的量使用组分(C)。只要组分(C)的量在该范围内,则避免固化不完全并且贮存稳定性令人满意。
(D)脱模剂
组分(D)为脱模剂,其选自由聚乙烯、有机硅化合物、氟化合物、脂肪酸、和脂肪酸酯组成的组,其可单独使用或者混合使用。其中,出于相容性,优选选择有机硅化合物。
适合的聚乙烯包括低分子量聚乙烯、低分子量聚乙烯共聚物、和通过上述物质的氧化改性或酸改性以引入极性基团而得到的改性聚乙烯蜡。该聚乙烯优选具有500-15,000、更优选地1,000-10,000的数均分子量(Mn),其通过使用四氢呋喃溶剂的GPC相对于聚苯乙烯标样测定。
聚乙烯蜡例如低分子量聚乙烯和低分子量聚乙烯共聚物可通过各种方法制备,例如在齐格勒(Ziegler)催化剂的存在下乙烯或者乙烯与α-烯烃的直接聚合、在高分子量聚乙烯或共聚物的制备过程中作为副产物的回收、或者高分子量聚乙烯或共聚物的热解。这些聚乙烯蜡中,优选由50-99mol%的乙烯和1-50mol%的α-烯烃组成的共聚物型聚乙烯蜡,更优选其中α-烯烃为聚丙烯的这些聚乙烯蜡。
氧化改性的聚乙烯蜡通过用过氧化物或氧处理聚乙烯蜡以在其中引入极性基团例如羧基或羟基而得到。酸改性的聚乙烯蜡通过任选地在过氧化物或氧的存在下用无机酸、有机酸或不饱和羧酸处理聚乙烯蜡以在其中引入极性基团例如羧基或磺酸而得到。这些聚乙烯蜡以普通高密度聚乙烯蜡、普通低密度聚乙烯蜡、低氧化型聚乙烯蜡、高氧化型聚乙烯蜡、酸改性的聚乙烯蜡、或者特殊单体改性的聚乙烯蜡的名称可商购得到并且可购自许多供应商。典型的实例包括蜡例如聚乙烯蜡和巴西棕榈蜡,脂肪酸例如硬脂酸及其金属盐。其中,出于接合性和脱模性,最优选巴西棕榈蜡。
适合的有机硅化合物包括聚二甲基硅氧烷的硅油、其中一些甲基被苯基替代的聚二甲基硅氧烷的硅油、其中一些甲基被氢或者两个以上碳原子的烷基替代的聚二甲基硅氧烷的硅油、其中一些甲基被卤代苯基替代的聚二甲基硅氧烷的硅油、其中一些甲基被氟代酯基替代的聚二甲基硅氧烷的硅油、环氧改性的硅油例如含有环氧基的聚二甲基硅氧烷、氨基改性的硅油例如含有氨基的聚二甲基硅氧烷、烷基-芳烷基硅油例如由二甲基硅氧烷和苯基甲基硅氧烷组成的硅油、聚醚改性的硅油例如其中二甲基硅氧烷单元中的一些甲基被聚醚替代的聚二甲基硅氧烷、和烷基-芳烷基聚醚改性的硅油例如其中二甲基硅氧烷单元中的一些甲基被聚醚替代的二甲基硅氧烷/苯基甲基硅氧烷聚合物。有机硅化合物应优选具有500-20,000、更优选地5,000-10,000的Mw。Mw太低的硅油将会蒸发并且引起对周围设备的污染,而Mw太高的硅油可能太粘稠以致无法处理。
适合的氟化合物包括含有3-40个碳原子、特别地5-20个碳原子的多氟代烷基或多氟代烷基醚基的化合物。例示性化合物包括C12F25NH3OOCC3H7、C3F7OC3H6Si(OCH3)3、和C8F17SC2H4COOH。
适合的脂肪酸包括至少12个碳原子的饱和脂肪酸和不饱和脂肪酸。脂肪酸的实例为月桂酸、十三酸、肉豆蔻酸、十五酸、棕榈酸、十七酸、硬脂酸、十九酸、花生酸、二十二酸、二十四酸、蜡酸、二十七酸、褐煤酸、三十酸、三十二酸、油酸、反油酸、亚油酸、亚麻酸、花生四烯酸、鲸蜡烯酸、和芥子酸。其中,优选C12-C22饱和脂肪酸。
适合的脂肪酸酯包括C5-C32脂肪酸与C2-C30一元醇或多元醇的酯。例示性脂肪酸包括饱和脂肪酸例如己酸、辛酸、十一酸、月桂酸、十三酸、肉豆蔻酸、棕榈酸、硬脂酸、二十二酸、二十四酸、蜡酸、褐煤酸、和三十酸;不饱和脂肪酸例如油酸、反油酸、亚油酸、亚麻酸、花生四烯酸、二十二烯酸、芥子酸、和蓖麻油酸。例示性醇包括一元醇例如丙醇、异丙醇、丁醇、辛醇、癸醇、月桂醇、肉豆蔻醇、硬脂醇、和二十二烷醇;和多元醇例如乙二醇、丙二醇、丁二醇、甘油、季戊四醇、和失水山梨醇。优选的脂肪酸酯为C12-C22脂肪酸与C2-C22一元醇或多元醇的酯。
相对于100重量份的组分(A)或者具有式(1)的树脂,以0.5-20重量份、优选地2-12重量份的量使用组分(D)。小于0.5重量份的组分(D)无法赋予脱模性或耐热性,存在使(用该膜保护的)衬底断裂的危险。大于20重量份的组分(D)导致低温区域中耐热性的降低,引起衬底表面的污染。
通过将该脱模剂与具有式(1)的树脂组合使用,从而使该树脂与待保护的衬底表面更相容。长期改善该膜与衬底的接合。该脱模剂的添加对于改善耐热性也有效。这是因为,脱模剂发挥缓和由树脂固化物的热膨胀引起的内部应力的功能以由此防止该膜从衬底表面剥离。
(E)阻燃剂
该树脂膜或树脂组合物可进一步包括(E)阻燃剂以防止燃烧。有机阻燃剂例如磷酸酯是适合的。
适合的磷酸酯包括亚磷酸、磷酸、亚膦酸、和膦酸的酯。
例示性亚磷酸酯包括亚磷酸三苯酯、亚磷酸三(壬基苯基)酯、亚磷酸三(2,4-二-叔-丁基苯基)酯、二硬脂基季戊四醇二亚磷酸酯、双(2,6-二-叔-丁基-4-甲基苯基)季戊四醇二亚磷酸酯、和双(2,4-二-叔-丁基苯基)季戊四醇二亚磷酸酯。
例示性磷酸酯包括磷酸三苯酯、磷酸三(壬基苯基)酯、磷酸三(2,4-二-叔-丁基苯基)酯、二硬脂基季戊四醇二磷酸酯、双(2,6-二-叔-丁基-4-甲基苯基)季戊四醇二磷酸酯、双(2,4-二-叔-丁基苯基)季戊四醇二磷酸酯、磷酸三丁酯、和双酚-A双(二苯基磷酸酯)。
亚膦酸酯的实例为四(2,4-二-叔-丁基苯基)-4,4'-亚联苯基亚膦酸酯。
膦酸酯的实例为二甲基苯膦酸酯和苯膦酸酯。
在磷酸酯中,优选亚磷酸酯、磷酸酯、和膦酸酯,最优选磷酸酯。
基于该表面保护膜,优选以0-40重量%的量、并且在使用时以0.1-40重量%、更优选地5-20重量%的量添加组分(E)。只要组分(E)的量在该范围内,则发挥所需的效果。阻燃剂可单独使用或者混合使用。
(F)抗氧化剂
该树脂膜或树脂组合物可进一步包括(F)抗氧化剂以改善热稳定性。该抗氧化剂优选为选自受阻酚化合物、受阻胺化合物、有机磷化合物、和有机硫化合物中的至少一种化合物。
尽管对本文中使用的受阻酚化合物并无特别限制,但优选以下列出的受阻酚化合物。
1,3,5-三甲基-2,4,6-三(3,5-二-叔-丁基-4-羟基苄基)苯(商品名:IRGANOX1330),
2,6-二-叔-丁基-4-甲基苯酚(商品名:Sumilizer BHT),
2,5-二-叔-丁基氢醌(商品名:Nocrac NS-7),
2,6-二-叔-丁基-4-乙基苯酚(商品名:Nocrac M-17),
2,5-二-叔-戊基氢醌(商品名:Nocrac DAH),
2,2'-亚甲基双(4-甲基-6-叔-丁基苯酚)(商品名:Nocrac NS-6),
3,5-二-叔-丁基-4-羟基苄基膦酸酯二乙酯(商品名:IRGANOX1222),
4,4'-硫代双(3-甲基-6-叔-丁基苯酚)(商品名:Nocrac 300),
2,2'-亚甲基双(4-乙基-6-叔-丁基苯酚)(商品名:Nocrac NS-5),
4,4'-亚丁基双(3-甲基-6-叔-丁基苯酚)(AdekaStab AO-40),
2-叔-丁基-6-(3-叔-丁基-2-羟基-5-甲基苄基)-4-甲基苯基丙烯酸酯(商品名:Sumilizer GM),
2-[1-(2-羟基-3,5-二-叔-戊基苯基)乙基]-4,6-二-叔-戊基苯基丙烯酸酯(商品名:Sumilizer GS),
2,2'-亚甲基双[4-甲基-6-(α-甲基环己基)苯酚],
4,4'-亚甲基双(2,6-二-叔-丁基苯酚)(商品名:Seenox 226M),
4,6-双(辛硫基甲基)-邻-甲酚(商品名:IRGANOX 1520L),
2,2'-亚乙基双(4,6-二-叔-丁基苯酚),
3-(3,5-二-叔-丁基-4-羟基苯基)丙酸十八烷基酯(商品名:IRGANOX 1076),
1,1,3-三(2-甲基-4-羟基-5-叔-丁基苯基)丁烷(商品名:Adeka Stab AO-30),
四[亚甲基-(3,5-二-叔-丁基-4-羟基氢化肉桂酸酯)]甲烷(商品名:Adeka StabAO-60),
三乙二醇双[3-(3-叔-丁基-5-甲基-4-羟基苯基)丙酸酯](商品名:IRGANOX245),
2,4-双(正-辛硫基)-6-(4-羟基-3,5-二-叔-丁基苯胺基)-1,3,5-三嗪(商品名:IRGANOX 565),
N,N'-六亚甲基双(3,5-二-叔-丁基-4-羟基氢化肉桂酰胺)(商品名:IRGANOX1098),
1,6-己二醇-双[3-(3,5-二-叔-丁基-4-羟基苯基)丙酸酯](商品名:IRGANOX259),
2,2-硫代-二亚乙基双[3-(3,5-二-叔-丁基-4-羟基苯基)丙酸酯](商品名:IRGANOX 1035),
3,9-双[2-[3-(3-叔-丁基-4-羟基-5-甲基苯基)丙酰氧基]-1,1-二甲基乙基]2,4,8,10-四氧杂螺[5.5]十一烷(商品名:Sumilizer GA-80),
三(3,5-二-叔-丁基-4-羟基苄基)异氰脲酸酯(商品名:IRGANOX 3114),
双(乙基3,5-二-叔-丁基-4-羟基苄基膦酸)钙/聚乙烯蜡50/50混合物(商品名:IRGANOX 1425WL),
3-(3,5-二-叔-丁基-4-羟基苯基)丙酸异辛酯(商品名:IRGANOX 1135),
4,4'-硫代双(6-叔-丁基-3-甲基苯酚)(商品名:Sumilizer WX-R),
6-[3-(3-叔-丁基-4-羟基-5-甲基苯基)丙氧基]-2,4,8,10-四-叔-丁基二苯并[d,f][1,3,2]二氧杂磷杂环庚烯(商品名:Sumilizer GP)等。
尽管对本文中使用的受阻胺化合物并无特别限制,但优选以下列出的受阻胺化合物。
对,对'-二辛基二苯基胺(商品名:IRGANOX 5057),
苯基-α-萘基胺(Nocrac PA),
聚(2,2,4-三甲基-1,2-二氢喹啉)(商品名:Nocrac 224,224-S),
6-乙氧基-2,2,4-三甲基-1,2-二氢喹啉(商品名:Nocrac AW),
N,N'-二苯基-对-苯二胺(商品名:Nocrac DP),
N,N'-二-β-萘基-对-苯二胺(商品名:Nocrac White),
N-苯基-N'-异丙基-对-苯二胺(商品名:Nocrac 810NA),
N,N'-二烯丙基-对-苯二胺(商品名:Nonflex TP),
4,4'-(α,α-二甲基苄基)二苯基胺(商品名:Nocrac CD),
对,对-甲苯磺酰基氨基二苯基胺(商品名:Nocrac TD),
N-苯基-N'-(3-甲基丙烯酰氧基-2-羟基丙基)-对-苯二胺(商品名:Nocrac G1),
N-(1-甲基庚基)-N'-苯基-对-苯二胺(商品名:Ozonon 35),
N,N'-二-仲-丁基-对-苯二胺(商品名:Sumilizer BPA),
N-苯基-N'-1,3-二甲基丁基-对-苯二胺(商品名:Antigene 6C),
烷基化的二苯基胺(商品名:Sumilizer 9A),
二甲基-1-(2-羟基乙基)-4-羟基-2,2,6,6-四甲基哌啶琥珀酸酯缩聚物(商品名:Tinuvin 622LD),
聚[[6-(1,1,3,3-四甲基丁基)氨基]-1,3,5-三嗪-2,4-二基][(2,2,6,6-四甲基-4-哌啶基)亚氨基]六亚甲基[(2,2,6,6-四甲基-4-哌啶基)亚氨基]](商品名:CHIMASSORB944),
N,N'-双(3-氨基丙基)乙二胺-2,4-双[N-丁基-N-(1,2,2,6,6-五甲基-4-哌啶基)氨基]-6-氯-1,3,5-三嗪缩合物(商品名:CHIMASSORB 119FL),
双(1-辛氧基-2,2,6,6-四甲基-4-哌啶基)癸二酸酯(商品名:Tinuvin 123),
双(2,2,6,6-四甲基-4-哌啶基)癸二酸酯(商品名:Tinuvin 770),
双(1,2,2,6,6-五甲基-4-哌啶基)2-(3,5-二-叔-丁基-4-羟基苄基)-2-正-丁基丙二酸酯(商品名:Tinuvin 144),
双(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯(商品名:Tinuvin 765),
四(1,2,2,6,6-五甲基-4-哌啶基)1,2,3,4-丁烷四羧酸酯(商品名:LA-57),
四(2,2,6,6-四甲基-4-哌啶基)1,2,3,4-丁烷四羧酸酯(商品名:LA-52),
1,2,3,4-丁烷四羧酸与1,2,2,6,6-五甲基-4-哌啶醇和1-十三醇的酯化混合物(商品名:LA-62),
1,2,3,4-丁烷四羧酸与2,2,6,6-四甲基-4-哌啶醇和1-十三醇的酯化混合物(商品名:LA-67),
1,2,3,4-丁烷四羧酸与1,2,2,6,6-五甲基-4-哌啶醇和3,9-双(2-羟基-1,1-二甲基乙基)-2,4,8,10-四氧杂螺[5.5]十一烷的酯化混合物(商品名:LA-63P),
1,2,3,4-丁烷四羧酸与2,2,6,6-四甲基-4-哌啶醇和3,9-双(2-羟基-1,1-二甲基乙基)-2,4,8,10-四氧杂螺[5.5]十一烷的酯化混合物(商品名:LA-68LD),
(2,2,6,6-四亚甲基-4-哌啶基)-2-丙烯羧酸酯(商品名:Adeka Stab LA-82),
(1,2,2,6,6-五甲基-4-哌啶基)-2-丙烯羧酸酯(商品名:Adeka Stab LA-87)等。
尽管对本文中使用的有机磷化合物并无特别限制,但优选以下列出的有机磷化合物。
双(2,4-二-叔-丁基苯基)[1,1-联苯]-4,4'-二基双亚磷酸酯,
9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(商品名:Sanko HCA),
亚磷酸三乙酯(商品名:JP302),
亚磷酸三正丁酯(商品名:JP304),
亚磷酸三苯酯(商品名:Adeka Stab TPP),
二苯基单辛基亚磷酸酯(商品名:Adeka Stab C),
亚磷酸三(对-甲苯基)酯(商品名:Chelex-PC),
二苯基单癸基亚磷酸酯(商品名:Adeka Stab 135A),
二苯基单(十三烷基)亚磷酸酯(商品名:JPM313),
亚磷酸三(2-乙基己基)酯(商品名:JP308),
苯基二癸基亚磷酸酯(商品名:Adeka Stab 517),
亚磷酸三癸酯(商品名:Adeka Stab 3010),
四苯基二丙二醇二亚磷酸酯(商品名:JPP100),
双(2,4-二-叔-丁基苯基)季戊四醇二亚磷酸酯(商品名:Adeka Stab PEP-24G),
亚磷酸三(十三烷基)酯(商品名:JP333E),
双(壬基苯基)季戊四醇二亚磷酸酯(商品名:Adeka Stab PEP-4C),
双(2,6-二-叔-丁基-4-甲基苯基)季戊四醇二亚磷酸酯(商品名:Adeka StabPEP-36),
双[2,4-二(1-苯基异丙基)苯基]季戊四醇二亚磷酸酯(商品名:Adeka Stab PEP-45),
三硫代亚磷酸三月桂酯(商品名:JPS312),
亚磷酸三(2,4-二-叔-丁基苯基)酯(商品名:IRGAFOS 168),
亚磷酸三(壬基苯基)酯(商品名:Adeka Stab 1178),
二硬脂基季戊四醇二亚磷酸酯(商品名:Adeka Stab PEP-8),
三(单、二壬基苯基)亚磷酸酯(商品名:Adeka Stab 329K),
亚磷酸三油醇酯(商品名:Chelex-OL),
亚磷酸三硬脂酯(商品名:JP318E),
4,4'-亚丁基双(3-甲基-6-叔-丁基苯基二(十三烷基))亚磷酸酯(商品名:JPH1200),
四(混合C12-C15烷基)-4,4'-亚异丙基二苯基二亚磷酸酯(商品名:Adeka Stab1500),
四(十三烷基)-4,4'-亚丁基双(3-甲基-6-叔-丁基苯基)二亚磷酸酯(商品名:Adeka Stab 260),
六(十三烷基)-1,1,3-三(2-甲基-5-叔-丁基-4-羟基苯基)丁烷三亚磷酸酯(商品名:Adeka Stab 522A),
氢化双酚A亚磷酸酯聚合物(HBP),
四(2,4-二-叔-丁基苯氧基)-4,4'-亚联苯基二膦(商品名:P-EPQ),
四(2,4-二-叔-丁基-5-甲基苯氧基)4,4'-亚联苯基二膦(商品名:GSY-101P),
2-[[2,4,8,10-四(1,1-二甲基乙基)二苯并[d,f][1,3,2]二氧杂磷杂环庚烯-6-基]氧]-N,N-双[2-[[2,4,8,10-四(1,1-二甲基乙基)二苯并[d,f][1,3,2]二氧杂磷杂环庚烯-6-基]氧]-乙基]乙胺(商品名:IRGAFOS 12),
2,2'-亚甲基双(4,6-二-叔-丁基苯基)辛基亚磷酸酯(商品名:Adeka Stab HP-10)等。
尽管对本文中使用的有机硫化合物并无特别限制,但优选以下列出的有机硫化合物。
3,3'-硫代二丙酸二月桂酯(商品名:Sumilizer TPL-R),
3,3'-硫代二丙酸二肉豆蔻酯(商品名:Sumilizer TPM),
3,3'-硫代二丙酸二硬脂酯(商品名:Sumilizer TPS),
季戊四醇四(3-十二烷基硫代丙酸酯)(商品名:Sumilizer TP-D),
3,3'-硫代二丙酸二(十三烷基)酯(商品名:Sumilizer TL),
2-巯基苯并咪唑(商品名:Sumilizer MB),
3,3'-硫代二丙酸二(十三烷基)酯(商品名:Adeka Stab AO-503A),
1,3,5-三-β-硬脂基硫代丙酰氧基乙基异氰脲酸酯,
3,3'-硫代二丙酸二(十二烷基)酯(商品名:IRGANOX PS 800FL),
3,3'-硫代二丙酸二(十八烷基)酯(商品名:IRGANOX PS 802FL)等。
上述抗氧化剂中,出于与用于形成树脂膜的组合物的溶剂和树脂(A)的相容性,特别优选受阻酚化合物。典型的受阻酚化合物为1,1,3-三(2-甲基-4-羟基-5-叔-丁基苯基)丁烷、十八烷基-3-(3,5-二-叔-丁基-4-羟基苯基)丙酸酯、异辛基-3-(3,5-二-叔-丁基-4-羟基苯基)丙酸酯、和4,6-双(辛硫基甲基)-邻-甲酚。
相对于100重量份的树脂(A),添加的组分(F)的适合量为0-5重量份,并且在使用时优选为0.1-5重量份,更优选为0.2-3重量份。只要组分(F)的量在该范围内,则发挥所需的效果并且确保相容性。
(G)填料
该树脂膜或树脂组合物可进一步包括(G)填料。其可以是任何公知的无机填料,例如,金属氧化物、金属氮化物、金属氢氧化物、和铁氧体。
适合的金属氧化物包括氧化锌、氧化铝、氧化镁、氧化硅、氧化铍、氧化铜和氧化亚铜。适合的金属氮化物包括氮化硼、氮化铝和氮化硅。适合的金属氢氧化物包括氢氧化镁、氢氧化钙、和氢氧化铝。典型的铁氧体为软磁铁氧体。也包括硅藻土、碱式硅酸镁、煅烧粘土、精细粉碎的二氧化硅、石英粉、结晶二氧化硅、高岭土、滑石、三氧化锑、精细粉碎的云母、二硫化钼、岩石棉、无机纤维(例如,陶瓷纤维、石棉)、和玻璃填料(例如,玻璃纤维、玻璃粉末、玻璃布、熔融石英)。
该无机填料可具有任意的各种形状,例如,颗粒、微颗粒、纳米颗粒、附聚物、大颗粒与细颗粒的复合颗粒、管、纳米管、线、棒、针、板、不定形、橄榄球、六面体、和液体。该无机填料可以是天然的或者合成的,并且可以单独使用或者混合使用。
优选地,该无机填料具有0.1-500μm、更优选地0.2-300μm、甚至更优选地0.5-50μm的平均粒径,该平均粒径为通过激光衍射法测量的中值直径。
该无机填料可以已用表面处理剂进行了表面处理。对该表面处理剂并无特别限制并且可以选自公知的试剂。适合的试剂包括硅烷偶联剂和钛酸酯偶联剂。
基于该表面保护膜,优选以0-50重量%的量、使用时以5-50重量%、更优选地10-30重量%、甚至更优选地15-20重量%的量添加组分(G)。只要组分(G)的量为该范围内,则固化膜不会有强度的显著降低并且消除了如下问题:剥离时使该膜破裂以使任意的树脂或添加剂残渣留在衬底上。
其他组分
该树脂膜或树脂组合物可进一步包括其他聚合物,只要该膜可接合于衬底,保持耐热性和耐压性,并且在工作结束时可顺利地剥离。适合的其他聚合物包括环氧树脂、聚烯烃树脂、双马来酰亚胺树脂、聚酰亚胺树脂、聚醚树脂、酚醛树脂、有机硅树脂、聚碳酸酯树脂、聚酰胺树脂、聚酯树脂、氟树脂、丙烯酸系树脂、蜜胺树脂、脲醛树脂、和聚氨酯树脂。使用时,相对于100重量份的该含有硅亚苯基-硅氧烷骨架的树脂(A),优选以0-1,000重量份的量添加其他树脂。
该树脂膜或树脂组合物可进一步包括其他添加剂,例如,增强剂、增稠剂、稳定剂、阻燃剂、颜料、着色剂、和助剂。相对于100重量份的含有硅亚苯基-硅氧烷骨架的树脂(A),优选以0-40重量份的量添加其他添加剂。
基膜
表面保护膜中包括的基膜是用于支承树脂膜的膜。其优选由聚酯、聚酰亚胺、聚酰胺、聚酰胺-酰亚胺、聚醚酰亚胺、三乙酸纤维素、聚醚砜或聚苯硫醚形成。该基膜可以是两个以上的膜层的层叠体。
适合的聚酯包括聚对苯二甲酸乙二醇酯(PET)、聚对苯二甲酸丁二醇酯(PBT)、和聚萘二甲酸乙二醇酯(PEN)。
尽管对基膜的厚度并无特别限制,但厚度优选为10-500μm,更优选为35-200μm。只要厚度在该范围内,该基膜就具有必要的最小刚度、施涂表面保护膜的充分的柔性、和加工的容易性。
表面保护膜的厚度,即基膜和树脂膜的总厚度优选为30-800μm,更优选为50-500μm,甚至更优选为100-300μm。具有至少30μm的厚度的表面保护膜足以填埋衬底上的凹凸,并且具有800μm以下的厚度的表面保护膜提供充分的导热性和对位标记的可视性。
表面保护膜的制备
本发明的另一实施方案为制备表面保护膜的方法,包括:将表面保护性树脂组合物施涂到基膜上的步骤,和将该组合物加热固化成树脂膜从而得到在该基膜上具有该树脂膜的表面保护膜的步骤。
通过将组分(A)-(D)和任选的组分溶解在溶剂中,从而得到该表面保护性树脂组合物。对用于配制该成膜树脂组合物的溶剂并无特别限制,只要有机组分可溶于其中。但是,具有极低沸点的溶剂在该组合物的制备过程中将会蒸发,对膜厚度产生不利的影响,而具有极高沸点的溶剂将会干扰膜形成。因此,建议使用具有60-180℃、更优选地80-140℃的沸点的溶剂。适合的溶剂包括癸烷、甲苯、二甲苯、四氢呋喃、环戊酮、醋酸乙酯、和异丙醇,但并不限于此。
尽管对使用的溶剂的量并无特别限制,但优选以使得该表面保护性树脂组合物可具有50-80重量%的固体浓度的量使用该溶剂。
可通过各种方法来制备该表面保护性树脂组合物。在使用混合器/振动器的一个方法中,将必要的组分供给到容器中,在容器中用振动器以500-4,000rpm将它们搅拌5-30分钟。在使用混合器的另一方法中,将必要的组分在溶剂中混合并溶解。在使用叶轮的又一方法中,将所有的组分供给到容器中,在容器中用叶轮对它们进行搅拌,或者使在容器中供给并搅拌一些组分或分成的部分的步骤顺次反复进行。
衬底加工层叠体
本发明的又一实施方案为衬底加工层叠体,其包括衬底和在该衬底的至少一个表面上设置的表面保护膜。该衬底加工层叠体可以例如通过使该表面保护膜附接于该衬底的至少一个表面而制备。一旦使该表面保护膜附接于该衬底的表面,则将该衬底的带有膜的表面保护。对该衬底的另一表面(与带有膜的表面相反)进行精密机加工或者将该层叠体移动或处理时,能够在没有对带有膜的衬底表面造成损伤或污染的情况下进行这样的操作。操作结束时,或者如果不再需要保护,于是能够在物理上将表面保护膜顺利地剥离。剥离后,在衬底表面上没有留下或留下很少的树脂和其他残渣。因此,实现操作效率和产量的显著改善。
本文中使用的衬底的实例包括硅系衬底例如硅晶片、氮化硅衬底、和氧化硅衬底;玻璃衬底例如玻璃晶片和石英衬底;塑料衬底例如酚醛纸、玻纤环氧树脂和聚酰亚胺衬底;印刷电路板、和其上具有配线或电极电路的有机衬底。
使该表面保护膜附接于该衬底中,可使用任何所需的工具,例如,真空层压机、压力型真空层压机、带式接合机或真空带式接合机。建议在附接之前将衬底预加热,原因在于使该表面保护膜与该衬底接触时,使该树脂膜软化并牢固地与衬底表面接触。一旦使该表面保护膜附接于衬底表面(待保护),则将该树脂膜加热固化。加热固化温度取决于催化剂的种类和量而变化,优选在60-220℃、更优选地100-210℃、甚至更优选地150-190℃的范围内选择。至少60℃的温度消除了问题例如长固化时间和固化不完全,而220℃以下的温度不会对衬底上的电路和该树脂组合物的物理性能产生不利影响。固化时间取决于催化剂的种类和量而变化,优选在0.25-10小时、更优选地0.5-6小时、甚至更优选地1-3小时的范围内选择。至少0.25小时的时间足以使该树脂组合物完全固化,而10小时以下的时间提供可接受的产量。
既然用本发明的表面保护膜将衬底保护,则在精密加工例如电路形成或TSV形成以及一般处理例如运输过程中,该膜用于防止对衬底表面上的通孔或电路以及衬底表面自身造成任何损伤和污染。本文中使用的术语“精密加工”包括电路形成、TSV形成、堆叠、旋涂、镀敷、干式蚀刻、等离子体处理等;并且术语“一般处理”包括进料、运输、临时贮存等。
将该表面保护膜从该衬底加工层叠体剥离时,可采用物理手段。例如,将刮刀插入该膜和衬底之间,并且利用该刮刀边缘作为起点将该膜与该衬底分离。然后,将该膜从该层叠体剥离而在衬底表面上没有留下残渣或污物。
实施例
以下通过例示而非通过限制给出本发明的实施例。通过使用四氢呋喃溶剂的GPC相对于聚苯乙烯标样测量树脂的Mw。通过1H-NMR波谱法分析树脂的组成。
以下示出实施例中使用的起始化合物S-1至S-7。
合成例1
在装备有搅拌器、温度计、氮吹扫管线和回流冷凝器的3-L烧瓶中,将14.3g的化合物S-1、477.0g的化合物S-2、和167.0g的化合物S-3溶解于2,000g的甲苯中并且在60℃下加热。然后将2.0g的催化剂(碳上的5wt%铂)放入该烧瓶中。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,在该温度下搅拌3小时,并且再次冷却到60℃。向该烧瓶中,放入2.0g的催化剂(碳上5wt%铂),并且历时0.5小时滴加44.9g的化合物S-4。在该过程中,内部温度上升到68℃。滴加结束时,将该反应溶液在90℃下熟化3小时。冷却到室温后,将700g的甲基异丁基酮(MIBK)添加到该反应溶液中,在压力下使其通过过滤器以除去铂催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将378g的环戊酮添加到残余物中,得到树脂A在环戊酮中的溶液,其具有65wt%的固体浓度。树脂A具有53,000的Mw。
树脂A
合成例2
在相似的3-L烧瓶中,将108.5g的化合物S-3和603.9g的化合物S-5溶解于2,040g的甲苯中并且在60℃下加热。然后将2.0g的催化剂(碳上的5wt%铂)放入该烧瓶中。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,在该温度下搅拌3小时,并且再次冷却到60℃。向该烧瓶中,放入2.0g的催化剂(碳上5wt%铂),并且历时0.5小时滴加23.3g的化合物S-4。在该过程中,内部温度上升到75℃。滴加结束时,将该反应溶液在90℃下熟化3小时。冷却到室温后,将700g的MIBK添加到该反应溶液中,在压力下使其通过过滤器以除去催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将396g的环戊酮添加到残余物中,得到树脂B的环戊酮溶液,其具有65wt%的固体浓度。树脂B具有53,900的Mw。
树脂B
合成例3
在相似的3-L烧瓶中,将86.8g的化合物S-3、603.9g的化合物S-5、和7.5g的化合物S-1溶解于1,950g的甲苯中并且在60℃下加热。然后将2.0g的催化剂(碳上的5wt%铂)放入该烧瓶中。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,在该温度下搅拌3小时,并且再次冷却到60℃。向该烧瓶中,放入2.0g的催化剂(碳上5wt%铂),并且历时0.5小时滴加23.3g的化合物S-4。在该过程中,内部温度上升到72℃。滴加结束时,将该反应溶液在90℃下熟化3小时。冷却到室温后,将700g的MIBK添加到该反应溶液中,在压力下使其通过过滤器以除去催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将388g的环戊酮添加到残余物中,得到树脂C的环戊酮溶液,其具有65wt%的固体浓度。树脂C具有62,200的Mw。
树脂C
合成例4
在相似的3-L烧瓶中,将252.3g的化合物S-6、318.5g的化合物S-7、和74.6g的化合物S-1溶解于1,950g的甲苯中并且在60℃下加热。然后将2.0g的催化剂(碳上的5wt%铂)放入该烧瓶中。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,在该温度下搅拌3小时,并且再次冷却到60℃。向该烧瓶中,放入2.0g的催化剂(碳上5wt%铂),并且历时0.5小时滴加77.8g的化合物S-4。在该过程中,内部温度上升到70℃。滴加结束时,将该反应溶液在90℃下熟化3小时。冷却到室温后,将700g的MIBK添加到该反应溶液中,在压力下使其通过过滤器以除去催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将389g的环戊酮添加到残余物中,得到树脂D的环戊酮溶液,其具有65wt%的固体浓度。树脂D具有32,000的Mw。
树脂D
合成例5
在装备有搅拌器、温度计、氮吹扫管线和回流冷凝器的3-L烧瓶中,将210.3g的化合物S-6、414.1g的化合物S-7、和37.3g的化合物S-1溶解于2,000g的甲苯中并且在60℃下加热。然后将2.0g的催化剂(碳上的5wt%铂)放入该烧瓶中。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,在该温度下搅拌3小时,并且再次冷却到60℃。向该烧瓶中,放入2.0g的催化剂(碳上的5wt%铂),并且历时0.5小时滴加101.1g的化合物S-4。在该过程中,内部温度上升到70℃。滴加结束时,将该反应溶液在90℃下熟化3小时。冷却到室温后,将700g的MIBK添加到该反应溶液中,在压力下使其通过过滤器以除去铂催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将410g的环戊酮添加到残余物中,得到树脂E的环戊酮溶液,其具有65wt%的固体浓度。树脂E具有25,000的Mw。
树脂E
比较合成例1
在相似的3-L烧瓶中,将27.1g的化合物S-3、629.1g的化合物S-5、和6.2g的化合物S-6溶解于1,950g的甲苯中并且在60℃下加热。然后将4.0g的催化剂(碳上的5wt%铂)放入该烧瓶中。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,并且在该温度下搅拌6小时。冷却到室温后,将700g的MIBK添加到该反应溶液中,在压力下使其通过过滤器以除去催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将356g的环戊酮添加到残余物中,得到树脂F的环戊酮溶液,其具有65wt%的固体浓度。树脂F具有50,100的Mw。
树脂F
比较合成例2
在相似的3-L烧瓶中,将542.7g的化合物S-3溶解于1,850g的甲苯中并且在60℃下加热。向该烧瓶中,将4.0g的催化剂(碳上的5wt%铂)放入并且滴加194.4g的化合物S-4。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,并且在该温度下搅拌3小时。冷却到室温后,将700g的MIBK添加到该反应溶液中,在压力下使其通过过滤器以除去催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将397g的环戊酮添加到残余物中,得到树脂G的环戊酮溶液,其具有65wt%的固体浓度。树脂G具有48,000的Mw。
树脂G
比较合成例3
在相似的3-L烧瓶中,将168.2g的化合物S-6、446.0g化合物S-7和37.3g的化合物S-1溶解于2,000g的甲苯中并且在60℃下加热。向该烧瓶中,放入2.0g的催化剂(碳上的5wt%铂)。确认内部温度上升到65-67℃,然后将该反应混合物在90℃下加热,并且在该温度下搅拌3小时,再次冷却到60℃。向该烧瓶中,放入2.0g的催化剂(碳上的5wt%铂),历经0.5小时滴加108.9g化合物S-4。在该过程中,内部温度上升到70℃。滴加结束时,将该反应溶液在90℃下熟化3小时。冷却到室温后,将700g的MIBK添加到该反应溶液中,在压力下使其通过过滤器以除去催化剂。将这样得到的聚合物溶液与600g的去离子水结合,搅拌,并且使其静置以静态分离,然后将下层或水层除去。将该分离和水洗工序反复进行6次,由此将痕量的酸成分从该聚合物溶液中除去。从该聚合物溶液中,在真空中将溶剂馏除。最后,将410g的环戊酮添加到残余物中,得到树脂H的环戊酮溶液,其具有65wt%的固体浓度。树脂H具有12,100的Mw。
树脂H
实施例1-10和比较例1-6
表面保护膜的制备
向每个树脂溶液中的100g树脂中,以与该树脂中的环氧基相当的量添加作为组分(B)的具有式(S-8)的三官能酚化合物(TrisP-PA,由Honshu Chemical Industry Co.,Ltd.生产)。向该溶液中添加0.5g的作为组分(C)的2-苯基-4-甲基-5-羟基甲基咪唑(ShikokuChemicals Corp.)、0.5g的抗氧化剂(Chimassorb944,由Ciba Specialty Chemicals生产)、作为组分(D)的表1中所示的脱模剂、和作为组分(G)的二氧化硅。采用刮刀将该溶液涂布到50μm厚的聚酰亚胺(PI)片上,并且在100℃下在干燥器中加热10分钟,在PI片上形成90μm厚的树脂膜。采用探针型厚度计测定该树脂膜的厚度。
Chimassorb944
Mn=2,000至3,100g/mol
表1
表1中,脱模剂KF-54为在25℃下具有450cSt的粘度的甲基苯基聚硅氧烷(Shin-Etsu Chemical Co.,Ltd.),Hi-wax为低分子量聚烯烃(Mitsui Chemicals,Inc.),并且Cheminox FA-4为2-(全氟丁基)乙醇(Unimatec Co.,Ltd.)。该填料为具有5.0μm的平均粒径的二氧化硅(Admatechs Co.)。
层合
使用真空层压机(TEAM-100,由TakatoriCorp.制造),在120℃下将该表面保护膜附接于硅晶片或玻璃晶片。使用带式接合机,在120℃下将该表面保护膜附接于有机衬底(玻纤-环氧树脂衬底)。在所有的情况下,在氮气氛中在180℃下将衬底上的膜加热4小时,由此使该树脂组合物固化,然后进行下述试验。
应指出的是,该硅晶片为在整个表面上分布有高10μm且直径40μm的铜柱的725μm厚的200mm硅晶片。该玻璃晶片为具有未加工的表面的200mm玻璃晶片。该有机衬底为一个表面上涂布有阻焊剂的15cm见方的玻纤-环氧树脂衬底。
接合试验
将接合于硅晶片、玻璃晶片或有机衬底的表面保护膜加热固化后,将其冷却并且目视检查界面接合状态。在界面处检测到气泡和缺陷时将该样品评价为差(×)并且在没有检测到缺陷时评价为良好(○)。
耐热性试验
将接合于硅晶片的表面保护膜加热固化后,将其放置在200℃或260℃下的热板上10分钟。将其冷却到室温并且目视检查界面接合状态。在界面处检测到气泡和缺陷时将该样品评价为差(×)并且在没有检测到缺陷时评价为良好(○)。
耐压性试验
将接合于硅晶片的表面保护膜加热固化后,将热和压力施加于该膜以考察是否由此使该树脂膜大幅地变形。对于热和压力的施加,在160℃的温度、10-3mbar的腔室内压、和5kN的载荷下使晶片接合机EVG520IS(EVG)运转。将该样品冷却到室温并且目视检查界面接合状态。在界面处检测到气泡和缺陷并且将树脂挤压到晶片侧边缘时将该样品评价为差(×)并且在没有缺陷也没有外侧挤压时评价为良好(○)。
剥离试验
通过真空抽吸将具有与硅晶片、玻璃晶片或有机衬底接合的(固化的)表面保护膜的层叠体设置在卡板上。通过用镊子拾取该膜并且提起镊子,从而在室温下将该表面保护膜剥离。当能够将该膜剥离而没有在衬底表面上留下树脂残渣或痕迹时将该样品评价为良好(○)并且当在衬底表面上留有树脂残渣或痕迹,不能将该膜剥离,或者由于附加的剥离力而在剥离过程中使该膜破裂时评价为差(×)。
长期贮存试验
将接合于硅晶片的表面保护膜加热固化后,使该层叠体冷却下来并且在室温下贮存15天或30天。目视检查该膜与衬底之间的界面状态。当贮存前后状态没有变化时将该样品评价为良好(○)并且在有任何变化时评价为差(×)。
通过真空抽吸将贮存15天或30天后的层叠体设置在卡板上。通过用镊子拾取该膜并且提起镊子,从而在室温下将该表面保护膜剥离。当能够将该膜剥离而没有在衬底表面上留下树脂残渣或痕迹时将该样品评价为良好(○)并且当在衬底表面上留有树脂残渣或痕迹,不能将该膜剥离,或者由于附加的剥离力而在剥离过程中使该膜破裂时评价为差(×)。
表2示出硅晶片上的表面保护膜的试验结果。表3示出玻璃晶片上的表面保护膜的试验结果。表4示出有机衬底上的表面保护膜的试验结果。
表2
表3
表4
由数据可以看到,本发明的表面保护膜在有用性能例如接合性、脱模能力和耐压性上令人满意,即使在长期贮存后也保持脱模能力,并且在衬底的加工和处理的过程中保护衬底表面。在加工结束时或者该表面保护膜停止其服务时,能够将该表面保护膜在物理上顺利地剥离而不需要任何特殊或昂贵的设备如UV照射设备,并且不会在衬底表面上留下任何树脂残渣或痕迹。
应指出的是,本发明并不限于上述的实施方案。这些实施方案只是例示性的,具有与下述权利要求中给出的技术思想基本上相同的构成并且发挥等同的功能和结果的任何实施方案被认为都在本发明的主旨和范围内。
通过引用将日本专利申请No.2016-019725并入本文中。
尽管已对一些优选的实施方案进行了说明,但根据上述教导可对其进行许多变形和改变。因此可理解,在不脱离所附权利要求的范围的情况下可在具体说明以外实施本发明。
Claims (11)
1.表面保护膜,其包括基膜和其上形成的树脂膜,所述树脂膜由树脂组合物形成,该树脂组合物包括组分(A)-(D):
(A)由式(1)表示并且具有10,000-100,000的重均分子量的含有硅亚苯基-硅氧烷骨架的树脂,
(B)能够与该含有硅亚苯基-硅氧烷骨架的树脂中的环氧基反应以形成交联结构的化合物,
(C)固化催化剂,和
(D)脱模剂,其选自由聚乙烯、具有500至20000的Mw的有机硅化合物和含有3-40个碳原子的多氟代烷基或多氟代烷基醚基的氟化合物组成的组,其量为0.5-20重量份,相对于100重量份的组分(A),
其中R1-R6各自独立地为C1-C20一价烃基或烷氧基,
a、b、c和d表示对应的重复单元的组成比,为满足以下条件的正数:0<a<1,0<b<1,0≤c<1,0<d<1,0.35≤a+c≤0.65,0.35≤b+d≤0.65,和a+b+c+d=1,g为0-300的整数,
X为具有式(2)的二价有机基团:
其中E为选自下述的二价有机基团:
s为0或1,R7和R8各自独立地为C1-C20一价烃基或烷氧基,t和u各自独立地为0-2的整数,并且
Y为具有式(3)的二价硅氧烷链:
其中R9-R14各自独立地为C1-C20一价烃基或烷氧基,并且j为0-300的整数。
2.根据权利要求1所述的表面保护膜,其中,式(1)中,a+c=0.5并且b+d=0.5。
3.根据权利要求1所述的表面保护膜,其中形成树脂膜的组合物还包括(E)阻燃剂、(F)抗氧化剂和(G)填料中的至少一种组分。
4.根据权利要求1所述的表面保护膜,其中该基膜由聚酯、聚酰亚胺、聚酰胺、聚酰胺-酰亚胺、聚醚酰亚胺、三乙酸纤维素、聚醚砜或聚苯硫醚形成。
5.根据权利要求1所述的表面保护膜,其中0<c<1。
6.衬底加工层叠体,其包括衬底和在该衬底的至少一个表面上设置的根据权利要求1所述的表面保护膜。
7.表面保护膜的制备方法,该表面保护膜包括基膜和其上形成的树脂膜,该方法包括:将表面保护性树脂组合物施涂到该基膜上的步骤、和将该组合物加热固化成该树脂膜的步骤,所述树脂组合物包括组分(A)-(D):
(A)由式(1)表示并且具有10,000-100,000的重均分子量的含有硅亚苯基-硅氧烷骨架的树脂,
(B)能够与该含有硅亚苯基-硅氧烷骨架的树脂中的环氧基反应以形成交联结构的化合物,
(C)固化催化剂,和
(D)脱模剂,其选自由聚乙烯、具有500至20000的Mw的有机硅化合物和含有3-40个碳原子的多氟代烷基或多氟代烷基醚基的氟化合物组成的组,其量为0.5-20重量份,相对于100重量份的组分(A),
其中R1-R6各自独立地为C1-C20一价烃基或烷氧基,
a、b、c和d表示对应的重复单元的组成比,为满足下述条件的正数:0<a<1,0<b<1,0≤c<1,0<d<1,0.35≤a+c≤0.65,0.35≤b+d≤0.65,和a+b+c+d=1,g为0-300的整数,
X为具有式(2)的二价有机基团:
其中E为选自下述的二价有机基团:
s为0或1,R7和R8各自独立地为C1-C20一价烃基或烷氧基,t和u各自独立地为0-2的整数,并且
Y为具有式(3)的二价硅氧烷链:
其中R9-R14各自独立地为C1-C20一价烃基或烷氧基,并且j为0-300的整数。
8.根据权利要求7所述的方法,其中,式(1)中,a+c=0.5并且b+d=0.5。
9.根据权利要求7所述的方法,其中该表面保护性树脂组合物还包括(E)阻燃剂、(F)抗氧化剂和(G)填料中的至少一种组分。
10.根据权利要求7所述的方法,其中该基膜由聚酯、聚酰亚胺、聚酰胺、聚酰胺-酰亚胺、聚醚酰亚胺、三乙酸纤维素、聚醚砜或聚苯硫醚形成。
11.保护具有电路形成表面的衬底的方法,包括:使根据权利要求1所述的表面保护膜附接于该衬底的电路形成表面的步骤,和将该树脂膜加热固化以使该表面保护膜与该衬底接合的步骤。
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