CN118117019A - 基于湿式处理的表面粗化方法 - Google Patents
基于湿式处理的表面粗化方法 Download PDFInfo
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- CN118117019A CN118117019A CN202410284855.5A CN202410284855A CN118117019A CN 118117019 A CN118117019 A CN 118117019A CN 202410284855 A CN202410284855 A CN 202410284855A CN 118117019 A CN118117019 A CN 118117019A
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- organic resin
- substrate
- layer
- surface roughening
- composition
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
-
- 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
- H01L21/02—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
- H01L21/18—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 the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
-
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Abstract
提供基板表面的粗化方法,包括:第1工序,在基板的表面上涂布含有无机粒子(a1)和有机树脂(a2)的组合物(a3),然后进行干燥和固化,从而在该基板上形成有机树脂层(A);第2工序,通过用含有氟化氢、过氧化氢或酸的溶液蚀刻形成了有机树脂层(A)的基板从而使该基板的表面粗化。优选蚀刻利用含有氟化氢和氟化铵、或过氧化氢和铵的溶液进行,有机树脂层(A)以相对于有机树脂(a2)100质量份无机粒子(a1)为5~50质量份的比例含有无机粒子(a1)和有机树脂(a2),组合物(a3)使用作为无机粒子(a1)的二氧化硅或氧化钛分散在有机溶剂中而得的二氧化硅溶胶或氧化钛溶胶、与有机树脂(a2)的溶液的混合物。
Description
本申请是申请日为2016年9月15日、申请号为201680052691.7、发明名称为“基于湿式处理的表面粗化方法”的专利申请的分案申请。
技术领域
本发明涉及基板上的表面粗化方法,该表面粗化方法可针对LED等的光取出层、太阳能电池的低反射玻璃进行。
背景技术
近年来,利用了LED技术。作为用于提高发光效率的技术,进行了以基于光取出层的光取出效率的提高为目标的研究。
作为前述光取出层,例如提出了在有机EL元件内部的发光层与基板之间设置光散射层的方法(参见专利文献1“微粒分散层”)。关于光散射层,可使用在透明的树脂中分散折射率与前述树脂不同的微粒而成的光散射层。利用发光部发出的光被光散射层散射,将前进方向变更为多个方向。多重散射的结果是,入射至空气界面的全反射角内的光被取出。为了使光散射层中光的前进方向无规则化,优选其中包含的微粒的尺寸分布宽,微粒的排列优选为无规则,另外,优选微粒的体积分率大。此处,若微粒的尺寸分布窄,或微粒的体积分率小,则光散射层的散射能力下降,无法充分实现其目的。然而,若微粒的尺寸分布过宽,则难以使微粒在树脂中理想地排列,另外,在微粒的尺寸分布宽的情况下,若使其体积分率过大,则光散射层的平坦性显著下降,由此,可能损害作为薄膜结构的发光部的平坦性,发光元件的可靠性大幅下降。
另外,作为高效率的光取出层,公开了具有反射层、和形成于前述反射层上的、包含变异系数为10%以下的微粒和折射率与前述微粒不同的基体的3维衍射层的光取出层(参见专利文献2)。该方式的特征在于,相对于3维衍射层的体积而言的前述微粒的体积分率为50%以上,而且,前述微粒在基体中排列而形成了具有短距离周期性的第一区域,进而,形成了该第一区域以无规则朝向相邻而集合的第二区域。
此外,对于已进行了实用化的太阳能电池而言,为了提高发光效率,实施了通过形成蜂巢结构等凸凹结构,从而降低反射率的技术。
现有技术文献
专利文献
专利文献1:日本特开2006-107744号公报
专利文献2:日本特开2009-216862号公报
发明内容
发明所要解决的课题
本发明提供使基板的表面粗化的方法。详细而言,提供下述方法:利用无机物与有机物的湿式蚀刻速度差,在基板上形成无机物和有机物混合存在的层,更具体而言,在基板的表面上由可被溶液蚀刻的无机物和无法被溶液蚀刻的有机物形成表面粗化形成层。接下来,通过利用溶液对无机物的存在部分进行蚀刻从而使基板的表面暴露,而且也对基板进行蚀刻,由此,使基板表面粗化的方法,例如能在基板上形成微细的凹凸的那样的粗化方法。
用于解决课题的手段
对于本发明而言,作为第1观点,为一种表面粗化方法,所述方法包括下述工序:第1工序,通过在基板的表面上涂布含有无机粒子(a1)和有机树脂(a2)的组合物(a3),然后进行干燥和固化,从而在该基板上形成有机树脂层(A);第2工序,通过用含有氟化氢、过氧化氢、或酸的溶液蚀刻形成了有机树脂层(A)的基板,从而使该基板的表面粗化。
作为第2观点,为第1观点所述的表面粗化方法,其中,蚀刻利用含有以下任一组的溶液进行:氟化氢和铵盐;过氧化氢和氨;过氧化氢和硫酸;磷酸和硝酸,
作为第3观点,为第1观点所述的表面粗化方法,其中,蚀刻利用含有氟化氢和氟化铵的溶液、或含有过氧化氢和氨的溶液进行,
作为第4观点,为第1观点~第3观点中任一项所述的表面粗化方法,其中,无机粒子(a1)为平均粒径5~1000nm的金属氧化物粒子,
作为第5观点,为第1观点所述的表面粗化方法,其中,组合物(a3)为作为无机粒子(a1)的二氧化硅分散在有机溶剂中而得的二氧化硅溶胶、或作为无机粒子(a1)的氧化钛分散在有机溶剂中而得的氧化钛溶胶、与有机树脂(a2)的溶液的混合物,
作为第6观点,为第1观点~第5观点中任一项所述的表面粗化方法,其中,有机树脂层(A)以相对于有机树脂(a2)100质量份而言无机粒子(a1)为5~70质量份的比例含有无机粒子(a1)和有机树脂(a2),
作为第7观点,为第1观点~第6观点中任一项所述的表面粗化方法,其中,有机树脂(a2)为具有重复单元结构的树脂,该重复单元结构包含在重复单元结构内具有羟基、羧基、氨基、缩水甘油基、或由它们的组合形成的官能团的结构,
作为第8观点,为第1观点~第7观点中任一项所述的表面粗化方法,其中,第2工序为通过蚀刻在基板表面形成高度直径比(高度)/(直径)在0.1~20的范围内的孔的工序,
作为第9观点,为第1观点~第8观点中任一项所述的表面粗化方法,其中,有机树脂层(A)为层厚0.001~10μm的层,
作为第10观点,为第1观点~第9观点中任一项所述的表面粗化方法,其中,第1工序在形成有机树脂层(A)之前还包括第1’工序,所述第1’工序中,通过在基板的表面上涂布含有有机树脂(b2)的组合物(b3),然后进行干燥和固化,从而在该基板上形成有机树脂层(B),
作为第11观点,为第10观点所述的表面粗化方法,其中,有机树脂(b2)选自有机树脂(a2),有机树脂(a2)是具有重复单元结构的树脂,该重复单元结构为在重复单元结构内具有羟基、羧基、氨基、缩水甘油基、或由它们的组合形成的官能团的结构,
作为第12观点,为第10观点或第11观点所述的表面粗化方法,其中,有机树脂层(B)为层厚0.001~10μm的层,
作为第13观点,为第1观点~第9观点中任一项所述的表面粗化方法,其中,组合物(a3)还含有交联剂和交联催化剂,
作为第14观点,为第10观点~第12观点中任一项所述的表面粗化方法,其中,组合物(a3)和组合物(b3)中的任一者或两者还含有交联剂和交联催化剂,
作为第15观点,为第1观点~第14观点中任一项所述的表面粗化方法,其中,在第2工序之后,还包括对基板表面进行气体蚀刻的第3工序,以及
作为第16观点,为将利用第1观点~第15观点中任一项所述的表面粗化方法形成的层作为LED的光取出层、或太阳能电池的低反射玻璃层使用的方法。
发明的效果
对于有机EL显示器而言,在玻璃、透明塑料等基板上形成ITO电极、空穴注入层、空穴传输层、发光层、电子传输层、电子注入层、电极。
另外,对于LED而言,在蓝宝石基板上形成N型半导体、发光域、P型半导体、ITO电极、SiO2层。
如上所述,为了提高它们的发光效率,对实现了光取出效率的提高的各种光取出层进行了研究。
此外,对于太阳能电池的转化效率的提高进行了研究,作为有效的方法,可举出抑制表面的太阳光反射的方法。
通过本发明的表面粗化方法,可使作为这些光取出层使用的玻璃、透明塑料、SiO2层等的表面粗化,例如形成微细的凹凸,因此,可降低该玻璃等处的光的反射,由此,使发光效率提高。本发明的表面粗化方法也可应用于在太阳能电池的反射降低层上形成微细的凸凹。
作为此前提出的降低光取出层中使用的基板的光的反射的方法,作为现有方法,有在光取出层中使用的基板上附着无机粒子等的方法,但无机粒子等在基板上的密合性成为问题。本发明与这些方法不同,通过将基板表面进行物理地蚀刻而使其粗化,例如形成凹凸等,不会发生现有方法中的基板与无机粒子等的密合性这样的问题。
需要说明的是,在进行基板表面的粗化时,利用光刻技术、干法蚀刻技术也能形成微细的凸凹,但存在装置昂贵、能制成的尺寸受限制这样的问题。
本发明中,包括下述工序:第1工序,通过在欲粗化的基板的表面上涂布含有无机粒子(a1)和有机树脂(a2)的组合物(a3),然后进行干燥和固化,从而在该基板上形成有机树脂层(A);和随后的第2工序,对形成了有机树脂层(A)的基板进行蚀刻,使基板的表面粗化。本发明中,利用有机树脂层(A)中包含的无机粒子(a1)与有机树脂(a2)的溶液的蚀刻的速度差,在有机树脂层(A)上形成凹凸的同时,详细而言,仅选择性地对有机树脂层(A)中包含的无机粒子(a1)的存在部分进行溶液蚀刻,从而基板表面暴露,SiO2等基板也被上述溶液蚀刻,因此形成凹凸。此处,上述有机树脂层(A)(尤其是有机树脂(a2))在进行溶液蚀刻方面发挥掩模的功能。
如上所述,本发明中,通过有机树脂层(A)的形成和随后的溶液蚀刻从而可容易地在基板表面形成微细的凹凸(进行粗化)。
需要说明的是,基板的粗化可通过无机粒子的平均粒径、有机树脂层(A)中包含的无机粒子的浓度(比例)而改变,可根据所需要的基板上的粗化形状(凹凸形状)来确定。
附图说明
图1为实施例1中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为30,000倍,有倾斜(tilt)。)。
图2为实施例2中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为10,000倍,有倾斜。)。
图3为实施例3中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为5,000倍,有倾斜。)。
图4为实施例4中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为30,000倍,有倾斜。)。
图5为实施例5中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为10,000倍,有倾斜。)。
图6为实施例6中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为30,000倍,有倾斜。)。
图7为实施例7中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为30,000倍,有倾斜。)。
图8为实施例8中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为30,000倍,有倾斜。)。
图9为实施例9中得到的形成有表面粗化形成层的SiO2膜被覆硅晶圆上的表面粗化图案的截面图(倍率为30,000倍,有倾斜。)。
具体实施方式
本发明涉及基板的表面粗化方法。
本说明书中,上述“粗化”是指利用蚀刻使基板表面***糙。通过利用化学处理或物理处理使基板表面发生变化,从而作为一个例子可在基板表面形成凹凸。
本发明是包括下述工序的表面粗化方法:第1工序,通过在基板的表面上涂布含有无机粒子(a1)和有机树脂(a2)的组合物(a3),然后进行干燥和固化,从而在该基板上形成有机树脂层(A);第2工序,通过用含有氟化氢、过氧化氢、或酸的溶液蚀刻形成了有机树脂层(A)的基板,从而使该基板的表面粗化。
前述第2工序中,可用优选含有氟化氢和铵盐的溶液、含有过氧化氢和氨的溶液、含有过氧化氢和硫酸的溶液、或含有磷酸和硝酸的溶液进行蚀刻。
例如可将含有氟化氢和铵盐的溶液制成缓冲溶液。
优选的方式中,蚀刻可用含有氟化氢和氟化铵的溶液、或含有过氧化氢和氨的溶液进行。
如上所述,本发明中,利用湿式蚀刻实施蚀刻。有机树脂层(A)中的无机粒子(a1)被前述的溶液蚀刻,另一方面,有机树脂层(A)中的有机树脂(a2)对于溶液显示耐蚀刻性。而且,在有机树脂层(A)的蚀刻到达基板面的阶段,可以接着用酸性水溶液对基板进行蚀刻。作为在上述酸性水溶液中使用的酸,可使用氢氟酸、硫酸、硝酸、盐酸、磷酸、缓冲的氢氟酸。
本发明中,用于蚀刻的溶液为水溶液,但还可含有有机溶剂。
有机溶剂为醇系、醚系、酮系或酯系。作为其具体例,可使用例如乙二醇单甲基醚、乙二醇单乙基醚、甲基溶纤剂乙酸酯、乙基溶纤剂乙酸酯、丙二醇单丁基醚、丙二醇单丁基醚乙酸酯、二乙二醇单甲基醚、二乙二醇单乙基醚、丙二醇、丙二醇单甲基醚、丙二醇单甲基醚乙酸酯、丙二醇单乙基醚、丙二醇单乙基醚乙酸酯、丙二醇丙基醚乙酸酯、甲苯、二甲苯、甲基乙基酮、环戊酮、环己酮、2-羟基丙酸乙酯、2-羟基-2-甲基丙酸乙酯、乙氧基乙酸乙酯、羟基乙酸乙酯、2-羟基-3-甲基丁酸甲酯、3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-乙氧基丙酸乙酯、3-乙氧基丙酸甲酯、丙酮酸甲酯、丙酮酸乙酯、乙酸乙酯、乙酸丁酯、乳酸乙酯、乳酸丁酯等。这些有机溶剂可单独使用,或者也可以以2种以上的组合的形式使用。
用于蚀刻的溶液中,水、或组合水和有机溶剂而成的全溶液中的铵盐、酸或氨的浓度为0.01~97质量%,全溶液中的过氧化氢的浓度为0.001~40质量%或0.01~40质量%。
例如,在过氧化氢与氨的混合溶液的情况下,可形成以NH4OH/H2O2/H2O=1:1:5~0.05:1:5的质量比例混合而成的水溶液。
例如,在过氧化氢与硫酸的混合溶液的情况下,可形成以H2SO4/H2O2=1:1~4:1的质量比例混合而成的水溶液。
例如,在使用氟化氢(酸)与氟化铵溶液的混合水溶液的情况下,可以以混合50质量%的氢氟酸水溶液、和40质量%的氟化铵水溶液而成的水溶液的形式使用。
作为本发明中使用的无机粒子(a1),可使用金属氧化物。可举出例如氧化硅(二氧化硅)、氧化钛、氧化锆、氧化铝、氮化硅、氮化钛等。特别优选氧化硅(二氧化硅)。作为平均粒径,可在5~1000nm、或5~200nm、或10~50nm的范围内使用。
这些无机粒子优选以胶体状态添加到有机树脂(a2)中,即,通过将在有机溶剂中分散上述无机粒子(a1)而成的溶胶添加到有机树脂(a2)或有机树脂(a2)的溶液中,可得到组合物(a3)。如后文所述,将该组合物(a3)用于基板的被覆。
典型地,使用作为无机粒子(a1)的二氧化硅分散在有机溶剂中而得的二氧化硅溶胶、或氧化钛分散在有机溶剂中而得的氧化钛溶胶,将这些溶胶与有机树脂(a2)的溶液混合,可得到组合物(a3)。
需要说明的是,本发明中,微粒的平均粒径是指用电子显微镜观察溶胶中的微粒而得到的值。
对于组合物(a3)、和通过涂布该组合物(a3)然后进行干燥和固化而得到的有机树脂层(A)而言,以相对于有机树脂(a2)100质量份而言、无机粒子(a1)为1~100质量份、或5~70质量份的比例含有无机粒子(a1)及有机树脂(a2)。
作为有机树脂(a2),优选的是,为具有重复单元结构的树脂,该重复单元结构为具有羟基、羧基、氨基、缩水甘油基、或由它们的组合形成的极性基团作为官能团的结构。这些官能团从与无机粒子的相容性、在基板上的涂布性方面考虑是优选的。另外,从固化膜变得不溶于酸性水溶液方面考虑,这些官能团也是优选的。
作为含有上述官能团的树脂,可举出丙烯酸系树脂、酚醛清漆系树脂等。
另外,作为有机树脂(a2),可使用聚醚及聚醚醚酮材料、环氧树脂。
作为丙烯酸系树脂,可举出:具有羟基、羧基、氨基或缩水甘油基的单体的均聚物、或它们与构成其他树脂的单体的共聚物。
作为前述单体,可举出(甲基)丙烯酸、(甲基)丙烯酸酯、乙烯基系化合物。
作为具有羟基、羧基、氨基或缩水甘油基的单体,可举出(甲基)丙烯酸、(甲基)丙烯酰胺、(甲基)丙烯酸羟基烷基酯、(甲基)丙烯酸羧基烷基酯、(甲基)丙烯酸氨基烷基酯、(甲基)丙烯酸缩水甘油酯、羟基苯乙烯、羟基乙烯基萘、苯甲酸乙烯酯等单体。
另外,作为构成其他树脂的单体,可举出不含上述官能团的单体,可举出例如(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯等(甲基)丙烯酸烷基酯、(甲基)丙烯酸苯酯、(甲基)丙烯酸苄酯、苯乙烯、叔丁基苯乙烯、乙烯基萘等。
这些丙烯酸系单体通过自由基聚合、阳离子聚合,可得到上述的丙烯酸系树脂。
作为聚醚和聚醚醚酮材料,可举出通过含有酚式羟基的化合物与含有卤素基的芳香族化合物的反应而得到的聚醚和聚醚醚酮。
作为酚醛清漆系树脂,可举出:通过含有酚式羟基的化合物或含有氨基的芳香族化合物、与醛化合物的反应而得的酚醛清漆树脂、通过含有酚式羟基的化合物或含有氨基的芳香族化合物、与含有羟基、羧基、或氨基的醛化合物的反应而得的酚醛清漆树脂。
作为具有酚式羟基的化合物,可举出苯酚、甲酚、水杨酸、萘酚等一元酚、邻苯二酚、间苯二酚等二元酚、连苯三酚、间苯三酚等三元酚、联苯酚、双酚A、双酚S等多核酚。
关于含有氨基的芳香族化合物,可举出吡咯、苯基萘基胺、苯基吲哚、咔唑、二苯基胺、3-羟基二苯基胺等。
作为醛类,可举出甲醛、多聚甲醛(paraformaldehyde)、乙醛、丙醛、丁醛、异丁醛、戊醛、己醛、2-甲基丁醛、2-乙基己基醛(2-乙基己醛)、己醛、十一烷醛、7-甲氧基-3,7-二甲基辛醛、环己醛、环己烷甲醛、3-甲基-2-丁醛、乙二醛、丙醛(malonaldehyde)、丙二醛(malondialdehyde)、丁二醛、戊二醛、己二醛等饱和脂肪族醛类、丙烯醛、甲基丙烯醛等不饱和脂肪族醛类、糠醛、吡啶醛等杂环式醛类、苯甲醛、萘甲醛、蒽甲醛、菲甲醛、水杨醛、苯基乙醛、3-苯基丙醛、甲苯甲醛、(N,N-二甲基氨基)苯甲醛、乙酰氧基苯甲醛等芳香族醛类等。
此外,可举出羟基、羧基、氨基键合于这些醛类而得到的醛类。
这些中,优选含有羟基或羧基的醛化合物,可举出例如羟基苯甲醛、羧基苯甲醛、羟基萘甲醛、羧基萘甲醛、羟基芘甲醛、羧基芘甲醛。
关于含有酚式羟基的化合物或含有氨基的芳香族化合物、与醛化合物,相对于苯基1当量,可以以0.1~10当量的比例使用醛类。
作为上述缩合反应中可使用的酸催化剂,可使用例如硫酸、磷酸、高氯酸等无机酸类、三氟甲磺酸、对甲苯磺酸、对甲苯磺酸一水合物等有机磺酸类、甲酸、草酸等羧酸类。酸催化剂的使用量可根据使用的酸类的种类而进行各种选择。通常,相对于含有酚式羟基的化合物或含有氨基的芳香族化合物、与醛化合物合计的100质量份而言,酸催化剂的使用量为0.001~10,000质量份,优选为0.01~1,000质量份,更优选为0.1~100质量份。
上述的缩合反应虽然可在无溶剂的情况下进行,但通常使用溶剂进行。作为溶剂,可使用所有溶剂,只要是不妨碍反应的溶剂即可。可举出例如丁基溶纤剂(2-丁氧基乙醇)等醚类、四氢呋喃、二氧杂环己烷等环状醚类。另外,使用的酸催化剂如果是例如甲酸那样的液状的物质,则也可使该酸催化剂兼有作为溶剂的作用。
缩合时的反应温度通常为40℃~200℃。反应时间可根据反应温度而进行各种选择,通常为30分钟~50小时左右。
作为本发明中使用的有机树脂(a2),可例举具有以下的式(1-1)~式(1-8)所示的重复单元结构的树脂。
另外,本发明中,除了上述的丙烯酸系树脂、酚醛清漆系树脂以外,可使用环氧树脂。
作为环氧树脂,可举出多官能环氧化合物,可使用例如丁烷四甲酸四(3,4-环氧环己基甲基)酯修饰ε-己内酯(株式会社ダイセル制,商品名エポリードGT401,脂环式环氧基)等。
对于本发明中使用的有机树脂(a2)而言,利用凝胶渗透色谱法(GPC)并按照聚苯乙烯换算而得到的重均分子量(Mw)为600~1,0000,00或600~200,000。
本发明中使用的组合物(a3)含有上述有机树脂(a2)、无机粒子(a1)和溶剂。根据需要可含有后述的表面活性剂等添加剂。
上述组合物(a3)中,可使固态成分相对于组合物(a3)的总质量而言为0.1~70质量%或0.1~60质量%。固态成分是指从构成组合物(a3)的全部成分中除去溶剂而剩余的成分。另外,可使有机树脂(a2)为相对于固态成分的总质量而言1~99.9质量%或20~99.9质量%的比例。
如上所述,本发明的表面粗化方法包括下述工序:
第1工序)通过在基板的表面上涂布含有无机粒子(a1)和有机树脂(a2)的组合物(a3),然后进行干燥和固化,从而在该基板上形成有机树脂层(A),以及
第2工序)通过用含有氟化氢、过氧化氢、或酸的溶液蚀刻形成了有机树脂层(A)的基板从而使该基板的表面粗化的工序,
进而,在第2工序之后,可包括:
第3工序)对基板表面进行气体蚀刻的工序。
即,本发明中,在基板上形成有机树脂层(A)后,从基板的上方进行蚀刻(湿式蚀刻、或湿式蚀刻和气体蚀刻),使基板的表面粗化。
另外,本发明的表面粗化方法中,第1工序在形成有机树脂层(A)之前还包括第1’工序,所述第1’工序中,通过在基板的表面上涂布含有有机树脂(b2)的组合物(b3),然后进行干燥和固化,从而在该基板上形成有机树脂层(B)。
本方式中,在基板上形成有机树脂层(B),在该有机树脂层(B)上形成有机树脂层(A)后,对基板进行蚀刻(湿式蚀刻、或湿式蚀刻与气体蚀刻),使基板的表面粗化。
在还包括第1’工序的情况下,有机树脂层(B)中包含的有机树脂(b2)为与上述有机树脂层(A)的有机树脂(a2)同样的范围的树脂,即,可从具有重复单元结构、且该重复单元结构为在重复单元结构内具有羟基、羧基、氨基、缩水甘油基、或由它们的组合形成的官能团的结构的有机树脂(a2)中选择。进而,有机树脂(b2)与有机树脂(a2)可使用相同的树脂。
本发明中使用的组合物(b3)含有上述有机树脂(b2)和溶剂。根据需要,可含有后述的表面活性剂等添加剂。
上述组合物(b3)中,可使固态成分相对于组合物(b3)的总质量而言为0.1~70质量%、或0.1~60质量%。固态成分是指从构成组合物(b3)的全部成分中除去溶剂而剩余的成分。另外,可使有机树脂(b2)为相对于固态成分的总质量而言1~100质量%、或1~99.9质量%、或50~99.9质量%的比例。
对于本发明中使用的有机树脂(b2)而言,利用凝胶渗透色谱法(GPC)并按照聚苯乙烯换算而得到的重均分子量(Mw)为600~1,000,000或600~200,000。
有机树脂层(B)可通过将组合物(b3)涂布在基板上、然后进行干燥和固化而得到,但由于在有机树脂层(B)的上层进一步涂布用于形成有机树脂层(A)的组合物(a3),因而为了防止混合(层混合),组合物(b3)可进一步含有交联剂和交联催化剂。
另外,根据需要,也可在形成有机树脂层(A)的组合物(a3)中含有交联剂和交联催化剂。
作为组合物(a3)或组合物(b3)中可使用的交联剂,可举出三聚氰胺系、取代脲系、或它们的聚合物系等。优选为具有至少2个交联形成取代基的交联剂,为甲氧基甲基化甘脲、丁氧基甲基化甘脲、甲氧基甲基化三聚氰胺、丁氧基甲基化三聚氰胺、甲氧基甲基化苯并胍胺、丁氧基甲基化苯并胍胺、甲氧基甲基化脲、丁氧基甲基化脲、甲氧基甲基化硫脲、或甲氧基甲基化硫脲等化合物。另外,也可使用这些化合物的缩合体。
交联剂的添加量根据使用的涂布溶剂、使用的基底基板、所要求的溶液粘度、所要求的膜形状等而变化,相对于组合物(a3)或组合物(b3)的全部固态成分的总质量而言,为0.001~80质量%,优选为0.01~50质量%,进一步优选为0.05~40质量%。
本发明中,作为用于促进上述交联反应的催化剂(交联催化剂),可配合对甲苯磺酸、三氟甲磺酸、对甲苯磺酸吡啶鎓、水杨酸、磺基水杨酸、柠檬酸、苯甲酸、羟基苯甲酸、萘甲酸等酸性化合物或/及2,4,4,6-四溴环己二烯酮、苯偶姻甲苯磺酸酯、甲苯磺酸2-硝基苄基酯、以及有机磺酸烷基酯等热产酸剂。
关于交联催化剂的配合量,相对于组合物(a3)或组合物(b3)的全部固态成分的总质量而言,为0.0001~20质量%,优选为0.0005~10质量%,优选为0.01~3质量%。
本发明中,作为组合物(a3)或组合物(b3)中可使用的表面活性剂,可举出例如聚氧乙烯月桂基醚、聚氧乙烯硬脂基醚、聚氧乙烯鲸蜡基醚、聚氧乙烯油基醚等聚氧乙烯烷基醚类、聚氧乙烯辛基苯酚醚、聚氧乙烯壬基苯酚醚等聚氧乙烯烷基芳基醚类、聚氧乙烯·聚氧丙烯嵌段共聚物类、山梨糖醇酐单月桂酸酯、山梨糖醇酐单棕榈酸酯、山梨糖醇酐单硬脂酸酯、山梨糖醇酐单油酸酯、山梨糖醇酐三油酸酯、山梨糖醇酐三硬脂酸酯等山梨糖醇酐脂肪酸酯类、聚氧乙烯山梨糖醇酐单月桂酸酯、聚氧乙烯山梨糖醇酐单棕榈酸酯、聚氧乙烯山梨糖醇酐单硬脂酸酯、聚氧乙烯山梨糖醇酐三油酸酯、聚氧乙烯山梨糖醇酐三硬脂酸酯等聚氧乙烯山梨糖醇酐脂肪酸酯类等非离子系表面活性剂、エフトップEF301、EF303、EF352((株)トーケムプロダクツ(现三菱マテリアル電子化成(株))制,商品名)、メガファックF171、F173、R-40(DIC(株)制,商品名)、フロラードFC430、FC431(住友スリーエム(株)制,商品名)、アサヒガードAG710、サーフロンSー382、SC101、SC102、SC103、SC104、SC105、SC106(旭硝子(株)制、商品名)等氟系表面活性剂、有机硅氧烷聚合物KP341(信越化学工业(株)制)等。
关于这些表面活性剂的配合量,相对于上述组合物(a3)或组合物(b3)的全部固态成分的总质量而言,通常为2.0质量%以下,优选为1.0质量%以下。这些表面活性剂可单独添加,或者也可以以2种以上的组合的形式添加。
本发明中,作为组合物(a3)或组合物(b3)中可使用的溶剂,可举出乙二醇单甲基醚、乙二醇单乙基醚、甲基溶纤剂乙酸酯、乙基溶纤剂乙酸酯、二乙二醇单甲基醚、二乙二醇单乙基醚、丙二醇、丙二醇单甲基醚、丙二醇单甲基醚乙酸酯、丙二醇单乙基醚、丙二醇单乙基醚乙酸酯、丙二醇丙基醚乙酸酯、甲苯、二甲苯、甲基乙基酮、甲基异丁基酮、环戊酮、环己酮、2-羟基丙酸乙酯、2-羟基-2-甲基丙酸乙酯、乙氧基乙酸乙酯、羟基乙酸乙酯、2-羟基-3-甲基丁酸甲酯、3-甲氧基丙酸甲酯、3-甲氧基丙酸乙酯、3-乙氧基丙酸乙酯、3-乙氧基丙酸甲酯、丙酮酸甲酯、丙酮酸乙酯、乙酸乙酯、乙酸丁酯、乳酸乙酯、乳酸丁酯等。这些有机溶剂可单独使用,或者以2种以上的组合使用。
进而,可混合使用丙二醇单丁基醚、丙二醇单丁基醚乙酸酯等高沸点溶剂。这些溶剂中,从提高流平性方面考虑,优选丙二醇单甲基醚、丙二醇单甲基醚乙酸酯、乳酸乙酯、乳酸丁酯、及环己酮等。
接下来,对本发明的表面粗化方法进行说明。
首先,利用使用了旋涂器(spinner)、涂布机(coater)等的适当的涂布方法,在基板或基材的表面上涂布组合物(a3),接着进行烘烤(干燥)而使其固化,在基板上制成有机树脂层(A)(第1工序)。另外,在包含有机树脂层(B)的情况下,首先,利用使用了旋涂器、涂布机等的适当的涂布方法,在基板或基材的表面上涂布组合物(b3),接着进行烘烤(干燥)而使其固化,在基板上制成有机树脂层(B)(第1’工序),然后,利用前述的步骤在该有机树脂层(B)上制成有机树脂层(A)即可。
本发明中,有机树脂层(A)优选为层厚0.001~10μm或0.005~3.0μm的层。另外,有机树脂层(B)优选为层厚0.001~10μm或0.005~3.0μm的层。
需要说明的是,上述有机树脂层(A)是通过后述的蚀刻对基板的表面的粗化形成有贡献的层,因此,本说明书中,也称为“表面粗化形成层”。
作为在涂布上述组合物(a3)或(b3)后进行烘烤的条件,为在80~400℃进行0.5~120分钟。
在基板上涂布组合物(a3)并在上述条件下使其固化而形成有机树脂层(A)后,针对形成了有机树脂层(A)的基板,详细而言,从该基板的上方利用前述的溶液进行蚀刻,由此,使基板的表面粗化(第2工序)。通过该湿式蚀刻,仅将该有机树脂层(A)中存在无机粒子(a1)的部分沿垂直方向削掉。在蚀刻到达基板面的阶段,也能接着用溶液对基板进行蚀刻,由此,在基板上形成凹凸而粗面化。
作为上述基板,不仅包括基板本身,还包括在基板上被覆SiO2等而成的被覆基板,可利用本发明的方法使基板的表面或被覆基板的表面粗化。
上述基于溶液的蚀刻(第2工序)进行至通过蚀刻而在基板表面形成高度直径比(高度)/(直径)在0.1~20的范围或0.1~10的范围的孔。通常,蚀刻时间为1秒~1小时或5秒~10分钟左右。作为基板,可举出例如硅、氧化硅、玻璃、蓝宝石等。
本发明中,不仅可利用湿式蚀刻,也可利用气体蚀刻(干法蚀刻)和湿式蚀刻这两者的组合进行。
例如,可按照下述方式进行:在基板上被覆地形成有机树脂层(B),在其上被覆地形成有机树脂层(A),首先,使用上述的溶液对有机树脂层(A)进行湿式蚀刻,然后,对有机树脂层(B)进行气体蚀刻而对基板进行加工。此处,气体蚀刻中,可使用四氟甲烷(CF4)、全氟环丁烷(C4F8)、全氟丙烷(C3F8)、三氟甲烷(CHF3)、二氟甲烷(CH2F2)、一氧化碳、氩、氧、氮、六氟化硫、三氟化氮及三氟化氯、氯、三氯硼烷及二氯硼烷等气体。
利用上述的本发明的表面粗化方法形成的层可作为LED的光取出层或太阳能电池的低反射玻璃层而合适地使用。
实施例
以下举出实施例进一步详细地说明本发明,但本发明不受它们的限制。
(合成例1)
将2-乙烯基萘30g、甲基丙烯酸缩水甘油酯3.5g、甲基丙烯酸1-丁氧基乙酯4.5g溶解于环己酮112g中,然后用氮气将烧瓶内置换,升温至60℃。升温后,在氮气加压下添加在环己酮48g中溶解的偶氮双异丁腈1.9g,于60℃反应24小时。将反应溶液冷却,然后投入至甲醇中,使聚合物再沉淀,进行加热干燥,得到具有前述式(1-1)表示的重复单元结构的聚合物。得到的聚合物的重均分子量Mw为6,000(按照聚苯乙烯换算)。式(1-1)中,将构成该聚合物的全部的重复单元结构的总数作为1.0时,由2-乙烯基萘形成的重复单元结构(数)所占的比例为0.8,由甲基丙烯酸缩水甘油酯形成的重复单元结构(数)所占的比例为0.1,由甲基丙烯酸1-丁氧基乙酯形成的重复单元结构(数)所占的比例为0.1。
(合成例2)
在100mL茄型烧瓶中装入二苯基胺(东京化成工业株式会社制)6.7g、3-羟基二苯基胺(东京化成工业株式会社制)7.3g、2-乙基己醛(东京化成工业株式会社制)10.2g、三氟甲磺酸(东京化成工业株式会社)0.8g、2-丁氧基乙醇(关东化学制)25.0g。然后用氮气将烧瓶内置换,然后进行加热,于150℃(回流状态)进行约1小时回流搅拌。反应结束后,用四氢呋喃(关东化学制)稀释至35质量%。将稀释液滴加至甲醇/氨水溶液(甲醇/水/氨=24/24/1)(体积比例)2000mL中,使其再沉淀。对得到的沉淀物进行抽滤,将滤得物用甲醇/氨水溶液(甲醇/水/氨=24/24/1)(体积比例)洗涤,然后于70℃进行一夜减压干燥,得到酚醛清漆树脂23.0g。得到的聚合物相当于具有前述式(1-8)表示的重复单元结构的聚合物。利用GPC并按照聚苯乙烯换算测得的重均分子量Mw为10,000。
(相当于组合物(a3)的表面粗化材料制备例1)
将合成例1中得到的树脂0.6g添加至有机二氧化硅溶胶液(日产化学工业株式会社制〔商品名〕MIBK-ST,分散介质为甲基异丁基酮,二氧化硅浓度为30质量%,平均粒径为10~15nm)0.02g、环己酮35.04g、丙二醇单甲基醚乙酸酯14.97g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-1)的溶液。
(相当于组合物(a3)的表面粗化材料制备例2)
将合成例1中得到的树脂0.6g添加至有机二氧化硅溶胶液(日产化学工业株式会社制〔商品名〕MIBK-ST-L,分散介质为甲基异丁基酮,二氧化硅浓度为30质量%,平均粒径为40~50nm)0.02g、环己酮24.61g、丙二醇单甲基醚乙酸酯10.51g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-2)的溶液。
(相当于组合物(a3)的表面粗化材料制备例3)
将合成例1中得到的树脂0.6g添加至有机二氧化硅溶胶液(日产化学工业株式会社制〔商品名〕MIBK-ST-ZL,分散介质为甲基异丁基酮,二氧化硅浓度为30质量%,平均粒径为70~100nm)0.02g、环己酮16.60g、丙二醇单甲基醚乙酸酯7.09g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-3)的溶液。
(相当于组合物(a3)的表面粗化材料制备例4)
将合成例1中得到的树脂0.3g添加至有机二氧化硅溶胶液(日产化学工业株式会社制〔商品名〕MIBK-ST,分散介质为甲基异丁基酮,二氧化硅浓度为30质量%,平均粒径为10~15nm)0.05g、环己酮18.22g、丙二醇单甲基醚乙酸酯7.77g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-4)的溶液。
(相当于组合物(a3)的表面粗化材料制备例5)
将合成例1中得到的树脂0.6g添加至有机二氧化硅溶胶液(日产化学工业株式会社制〔商品名〕MIBK-ST-L,分散介质为甲基异丁基酮,二氧化硅浓度为30质量%,平均粒径为40~50nm)0.1g、环己酮29.06g、丙二醇单甲基醚乙酸酯12.37g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-5)的溶液。
(相当于组合物(a3)的表面粗化材料制备例6)
将合成例1中得到的树脂0.3g添加至有机二氧化硅溶胶液(日产化学工业株式会社制〔商品名〕MIBK-ST-L,分散介质为甲基异丁基酮,二氧化硅浓度为30质量%,平均粒径为40~50nm)0.1g、环己酮25.52g、丙二醇单甲基醚乙酸酯10.87g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-6)的溶液。
(相当于组合物(a3)的表面粗化材料制备例7)
将合成例1中得到的树脂0.3g添加至有机二氧化硅溶胶液(日产化学工业株式会社制〔商品名〕PGM-ST,分散介质为丙二醇单甲基醚,二氧化硅浓度为30质量%,平均粒径为10~15nm)0.05g、环己酮18.22g、丙二醇单甲基醚乙酸酯7.78g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-7)的溶液。
(相当于组合物(a3)的表面粗化材料制备例8)
将作为有机树脂(a2)的商品名エポリードGT401(株式会社ダイセル化学制)0.3g添加至有机二氧化硅溶胶液(日产化学工业株式会社制,商品名MIBK-ST,分散介质为甲基异丁基酮,二氧化硅浓度为30质量%,平均粒径为10~15nm)0.5g、丙二醇单甲基醚乙酸酯48.78g、丙二醇单甲基醚0.1g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-8)的溶液。
(相当于组合物(a3)的表面粗化材料制备例9)
将合成例2中得到的树脂0.30g添加至サンコロイド液(日产化学工业株式会社制,商品名HT-R305M7-20,氧化钛溶胶,分散介质为甲醇,氧化钛浓度为30质量%,平均粒径为20~25nm)0.15g、丙二醇单甲基醚16.26g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备组合物(a3-9)的溶液。
(比较制备例1)
将合成例1中得到的树脂0.6g添加至环己酮29.06g、丙二醇单甲基醚乙酸酯12.37g中,制成溶液。然后,使用孔径为0.2μm的聚乙烯制微滤器进行过滤,制备比较组合物(a3-10)的溶液。
<表面粗化形成层的形成>
实施例1
利用旋涂机,将表面粗化材料制备例1中得到的组合物(a3-1)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了15nm的有机树脂层A(表面粗化形成层)。
实施例2
利用旋涂机,将表面粗化材料制备例2中得到的组合物(a3-2)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了40nm的有机树脂层A(表面粗化形成层)。
实施例3
利用旋涂机,将表面粗化材料制备例3中得到的组合物(a3-3)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了90nm的有机树脂层A(表面粗化形成层)。
实施例4
利用旋涂机,将表面粗化材料制备例4中得到的组合物(a3-4)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了15nm的有机树脂层A(表面粗化形成层)。
实施例5
利用旋涂机,将表面粗化材料制备例5中得到的组合物(a3-5)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了40nm的有机树脂层A(表面粗化形成层)。
实施例6
利用旋涂机,将表面粗化材料制备例6中得到的组合物(a3-6)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了40nm的有机树脂层A(表面粗化形成层)。
实施例7
利用旋涂机,将表面粗化材料制备例7中得到的组合物(a3-7)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了15nm的有机树脂层A(表面粗化形成层)。
实施例8
利用旋涂机,将表面粗化材料制备例5中得到的组合物(a3-5)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了40nm的有机树脂层A(表面粗化形成层)。
实施例9
利用旋涂机,将表面粗化材料制备例8中得到的组合物(a3-8)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了15nm的有机树脂层A(表面粗化形成层)。
实施例10
利用旋涂机,将表面粗化材料制备例9中得到的组合物(a3-9)的溶液涂布于TiN基板,于300℃进行1分钟烧成,形成了15nm的有机树脂层A(表面粗化形成层)。
比较例1
利用旋涂机,将比较制备例1中得到的比较组合物(a3-10)的溶液涂布于TEOS基板(SiO2膜被覆硅晶圆),于240℃进行1分钟烧成,形成了40nm的有机树脂层A(表面粗化形成层)。
(表面粗化评价)
用商品名LAL1400(ステラケミファ社制,氢氟酸与氟化铵溶液的混合水溶液)对由实施例1~9得到的形成有有机树脂层A(表面粗化形成层)的晶圆进行蚀刻。在烧杯中储存LAL1400后,浸渍该晶圆而实施蚀刻。用15~240秒的蚀刻时间进行。然后,为了将残留在晶圆上的有机物残渣除去,利用RIE-10NR(サムコ株式会社),使用O2气体进行灰化除去。
用氨/过氧化氢/水=25/100/500对由实施例10得到的形成有有机树脂层A(表面粗化形成层)的晶圆进行蚀刻。在烧杯中储存上述溶液后,将烧杯浸于热水浴中加热至50℃。然后,将该晶圆浸渍于该溶液中而实施蚀刻。用60秒的蚀刻时间进行。然后,为了将残留在晶圆上的有机物残渣除去,利用RIE-10NR(サムコ株式会社),使用O2气体进行灰化除去。
另外,对于由比较例1得到的有机树脂层(表面粗化形成层),与实施例1~9同样地进行蚀刻和灰化除去。
对由实施例1~9得到的形成有表面粗化形成层的晶圆进行蚀刻、灰化除去,对于使表面进行了粗化的晶圆,针对其表面,使用扫描型电子显微镜(Hitachi S-4800),观察表面粗化图案形状(参见图1~图9)。
[表1]
表1表面粗化形成层的形状观察
产业上的可利用性
本发明提供使基板的表面粗化的方法。详细而言,利用无机物与有机物的溶液的蚀刻速度差,在基板上形成无机物和有机物混合存在的层,更具体而言,在基板的表面上形成可被溶液蚀刻的部分和无法被溶液蚀刻的部分混合存在的表面粗化形成层。接下来,通过利用溶液对无机物存在的部分进行蚀刻,从而使基板的表面暴露,与此同时,SiO2被覆基板也通过溶液的蚀刻而发生表面粗化,由此,例如能在基板上形成微细的凹凸。利用这些,本发明的表面粗化方法可应用于LED等的光取出层或太阳能电池的低反射层的形成。
Claims (17)
1.一种表面粗化方法,所述方法包括下述工序:
第1工序,通过在基板的表面上涂布含有在有机溶剂中分散无机粒子a1而成的溶胶和有机树脂a2的组合物a3,然后进行干燥和固化,从而在该基板上形成有机树脂层A;
第2工序,通过用含有氟化氢、过氧化氢、或酸的溶液蚀刻形成了有机树脂层A的基板,从而有机树脂层A中的无机粒子a1被蚀刻,使该基板的表面粗化。
2.如权利要求1所述的表面粗化方法,在第2工序中,在有机树脂层A中的无机粒子a1被蚀刻而到达基板面的阶段,接着用所述溶液对该基板进行蚀刻,使该基板的表面粗化。
3.如权利要求1所述的表面粗化方法,其中,蚀刻利用含有以下任一组的溶液进行:
氟化氢和铵盐;过氧化氢和氨;过氧化氢和硫酸;磷酸和硝酸。
4.如权利要求1所述的表面粗化方法,其中,蚀刻利用含有氟化氢和氟化铵的溶液、或含有过氧化氢和氨的溶液进行。
5.如权利要求1所述的表面粗化方法,其中,无机粒子a1是平均粒径为5~1000nm的金属氧化物粒子。
6.如权利要求1所述的表面粗化方法,其中,组合物a3为作为无机粒子a1的二氧化硅分散在有机溶剂中而得的二氧化硅溶胶、或作为无机粒子a1的氧化钛分散在有机溶剂中而得的氧化钛溶胶、与有机树脂a2的溶液的混合物。
7.如权利要求1所述的表面粗化方法,其中,有机树脂层A以相对于100质量份有机树脂a2而言、无机粒子a1为5~70质量份的比例含有无机粒子a1和有机树脂a2。
8.如权利要求1所述的表面粗化方法,其中,有机树脂a2为具有重复单元结构的树脂,该重复单元结构包含具有羟基、羧基、氨基、缩水甘油基、或由它们的组合形成的官能团的结构。
9.如权利要求1所述的表面粗化方法,其中,第2工序为通过蚀刻在基板表面形成高度直径比(高度)/(直径)在0.1~20范围内的孔的工序。
10.如权利要求1所述的表面粗化方法,其中,有机树脂层A为层厚0.001~10μm的层。
11.如权利要求1所述的表面粗化方法,其中,第1工序在形成有机树脂层A之前还包括第1’工序,所述第1’工序中,通过在基板的表面上涂布含有有机树脂b2的组合物b3,然后进行干燥和固化,从而在该基板上形成有机树脂层B。
12.如权利要求11所述的表面粗化方法,其中,有机树脂b2选自有机树脂a2,有机树脂a2是具有重复单元结构的树脂,该重复单元结构为在重复单元结构内具有羟基、羧基、氨基、缩水甘油基、或由它们的组合形成的官能团的结构。
13.如权利要求11所述的表面粗化方法,其中,有机树脂层B为层厚0.001~10μm的层。
14.如权利要求1所述的表面粗化方法,其中,组合物a3还含有交联剂和交联催化剂。
15.如权利要求11所述的表面粗化方法,其中,组合物a3和组合物b3中的任一者或两者还含有交联剂和交联催化剂。
16.如权利要求1~15中任一项所述的表面粗化方法,其中,在第2工序之后,还包括对基板表面进行气体蚀刻的第3工序。
17.将利用权利要求1~16中任一项所述的表面粗化方法形成的层作为LED的光取出层或太阳能电池的低反射玻璃层使用的方法。
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