CN116330766A - 层叠体、带有机硅树脂层的支撑基材、带有机硅树脂层的树脂基板、电子器件的制造方法 - Google Patents
层叠体、带有机硅树脂层的支撑基材、带有机硅树脂层的树脂基板、电子器件的制造方法 Download PDFInfo
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- CN116330766A CN116330766A CN202310250134.8A CN202310250134A CN116330766A CN 116330766 A CN116330766 A CN 116330766A CN 202310250134 A CN202310250134 A CN 202310250134A CN 116330766 A CN116330766 A CN 116330766A
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- resin layer
- silicone resin
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- laminate
- glass
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- 238000000034 method Methods 0.000 title abstract description 78
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 61
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- 230000006866 deterioration Effects 0.000 abstract description 30
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Abstract
本发明涉及层叠体、带有机硅树脂层的支撑基材、带有机硅树脂层的树脂基板、电子器件的制造方法,提供一种抑制了有机硅树脂层的端部变质的层叠体,其依次具备支撑基材、有机硅树脂层和基板,有机硅树脂层包含选自由3d过渡金属、4d过渡金属、镧系金属及铋组成的组中的至少1种金属元素。
Description
本申请是申请日为2017年12月26日、申请号为201711435275.8、发明名称为“层叠体、带有机硅树脂层的支撑基材、带有机硅树脂层的树脂基板、电子器件的制造方法”的申请的分案申请。
技术领域
本发明涉及层叠体、带有机硅树脂层的支撑基材、带有机硅树脂层的树脂基板、及电子器件的制造方法。
背景技术
近年来,太阳能电池(PV)、液晶面板(LCD)、有机EL面板(OLED)、感知电磁波、X射线、紫外线、可见光线、红外线等的接收传感器面板等器件(电子设备)正逐渐薄型化、轻量化,这些器件中使用的以玻璃基板为代表的基板正逐渐薄板化。若因薄板化而基板的强度不足,则在器件的制造工序中,基板的处理性降低。
最近,为了应对上述的问题,提出了如下方法:准备将玻璃基板和加强板层叠而成的玻璃层叠体,在玻璃层叠体的玻璃基板上形成显示装置等电子器件用构件后,将加强板从玻璃基板分离的方法(例如,专利文献1)。加强板具有支撑板和固定于该支撑板上的有机硅树脂层,在玻璃层叠体中,有机硅树脂层与玻璃基板可剥离地密合。
现有技术文献
专利文献
专利文献1:国际公开第2007/018028号
发明内容
发明要解决的问题
近年来,随着电子器件用构件的高功能化、复杂化,期望在形成氧化物半导体等电子器件用构件时,在大气气氛下、在更高温条件(例如450℃)下实施加热处理。
本发明人等准备专利文献1中记载的玻璃层叠体并实施了在上述条件下的加热处理,结果发现玻璃层叠体中的有机硅树脂层的端部附近发生白化、发生变质(以后,将这样的变质也称为“端部变质”)。具体而言,如实施了加热处理的玻璃层叠体的俯视图即图3所示,在玻璃层叠体100的有机硅树脂层的端部102发生变质。若伴着这样的端部变质在有机硅树脂层的端部附近产生间隙,则容易产生如下工艺上的不良情况:湿法工序中所使用的化学试剂浸入至玻璃层叠体中,污染其后实施的真空工艺装置;前工序的药剂混入至其它湿法工序中所使用的药剂中等。
本发明鉴于上述实际情况,提供抑制了有机硅树脂层的端部变质的层叠体。
另外,本发明还提供能够适用于上述层叠体的带有机硅树脂层的支撑基材、带有机硅树脂层的树脂基板、及电子器件的制造方法。
用于解决问题的方案
本发明人等为了解决上述问题而进行了深入研究,结果发现,通过以下的构成能够解决上述课题。
(1)一种层叠体,其依次具备支撑基材、有机硅树脂层和基板,
有机硅树脂层包含选自由3d过渡金属、4d过渡金属、镧系金属及铋组成的组中的至少1种金属元素。
(2)根据(1)所述的层叠体,其中,有机硅树脂层包含选自由3d过渡金属、镧系金属及铋组成的组中的至少1种金属元素。
(3)根据(1)或(2)所述的层叠体,其中,有机硅树脂层包含选自由铁、锰、铜、铈、钴、镍、铬及铋组成的组中的至少1种金属元素。
(4)根据(1)~(3)中任一项所述的层叠体,其中,有机硅树脂层包含选自由铁、锰、铜、铈及铋组成的组中的至少1种金属元素。
(5)根据(1)~(4)中任一项所述的层叠体,其中,多个基板夹着有机硅树脂层层叠于支撑基材上。
(6)根据(1)~(5)中任一项所述的层叠体,其中,基板为玻璃基板。
(7)根据(1)~(5)中任一项所述的层叠体,其中,基板为树脂基板。
(8)根据(7)所述的层叠体,其中,树脂基板为聚酰亚胺树脂基板。
(9)根据(1)~(5)中任一项所述的层叠体,其中,基板为包含半导体材料的基板。
(10)根据(9)所述的层叠体,其中,半导体材料为Si、SiC、GaN、氧化镓、或金刚石。
(11)一种带有机硅树脂层的支撑基材,其依次具备支撑基材和有机硅树脂层,
有机硅树脂层包含选自由3d过渡金属、4d过渡金属、镧系金属及铋组成的组中的至少1种金属元素。
(12)一种电子器件的制造方法,其具备:
构件形成工序,在(1)~(10)中任一项所述的层叠体的基板的表面上形成电子器件用构件,得到带电子器件用构件的层叠体;和
分离工序,从带电子器件用构件的层叠体将包含支撑基材及有机硅树脂层的带有机硅树脂层的支撑基材去除,得到具有基板和电子器件用构件的电子器件。
(13)一种带有机硅树脂层的树脂基板,其依次具备树脂基板和有机硅树脂层,
有机硅树脂层包含选自由3d过渡金属、4d过渡金属、镧系金属及铋组成的组中的至少1种金属元素。
(14)一种电子器件的制造方法,其具备:
形成层叠体的工序,使用(13)所述的带有机硅树脂层的树脂基板和支撑基材形成层叠体;
构件形成工序,在层叠体的树脂基板的表面上形成电子器件用构件,得到带电子器件用构件的层叠体;及
分离工序,从带电子器件用构件的层叠体去除支撑基材及有机硅树脂层,得到具有树脂基板和电子器件用构件的电子器件。
发明的效果
根据本发明,能够提供抑制了有机硅树脂层的端部变质的层叠体。
另外,根据本发明,可以提供能够应用于上述层叠体的带有机硅树脂层的支撑基材、带有机硅树脂层的树脂基板及电子器件的制造方法。
附图说明
图1为本发明的玻璃层叠体的一个实施方式的示意性截面图。
图2的(A)及图2的(B)为依照工序顺序示出本发明的电子器件的制造方法的一个实施方式的示意性截面图。
图3为示出以往的层叠体中发生端部变质的状况的俯视图。
附图标记说明
10、100 玻璃层叠体
12 支撑基材
14 有机硅树脂层
14a 有机硅树脂层的表面
16 玻璃基板
16a 玻璃基板的第1主面
16b 玻璃基板的第2主面
18 带树脂层的支撑基材
20 电子器件用构件
22 带电子器件用构件的层叠体
24 带构件的玻璃基板
102 端部
L 端部变质长度
具体实施方式
以下,参照附图对用于实施本发明的方式进行说明,但本发明不限制于以下的实施方式,只要不脱离本发明的范围,则可以对以下的实施方式施加各种变形及置换。
图1为作为本发明的层叠体的一个方式的玻璃层叠体的一个实施方式的示意性截面图。
如图1所示,玻璃层叠体10为包含支撑基材12及玻璃基板16、以及配置于它们之间的有机硅树脂层14的层叠体。对于有机硅树脂层14,其一个面与支撑基材12接触、并且其另一面与玻璃基板16的第1主面16a接触。
玻璃层叠体10中,有机硅树脂层14与玻璃基板16之间的剥离强度低于有机硅树脂层14与支撑基材12之间的剥离强度,有机硅树脂层14与玻璃基板16剥离,分离为有机硅树脂层14及支撑基材12的层叠体、和玻璃基板16。换言之,有机硅树脂层14固定于支撑基材12上,玻璃基板16可剥离地层叠于有机硅树脂层14上。
包含支撑基材12及有机硅树脂层14的2层部分具有对玻璃基板16进行加强的功能。需要说明的是,将为了制造玻璃层叠体10而预先制造的包含支撑基材12及有机硅树脂层14的2层部分称为带有机硅树脂层的支撑基材18。
该玻璃层叠体10通过后述的步骤分离为玻璃基板16和带有机硅树脂层的支撑基材18。带有机硅树脂层的支撑基材18可以与新的玻璃基板16层叠,作为新的玻璃层叠体10再利用。
支撑基材12与有机硅树脂层14之间的剥离强度为剥离强度(x),若在支撑基材12与有机硅树脂层14之间施加超过剥离强度(x)的剥离方向的应力,则支撑基材12与有机硅树脂层14剥离。有机硅树脂层14与玻璃基板16之间的剥离强度为剥离强度(y),若在有机硅树脂层14与玻璃基板16之间施加超过剥离强度(y)的剥离方向的应力,则有机硅树脂层14与玻璃基板16剥离。
玻璃层叠体10中,上述剥离强度(x)高于上述剥离强度(y)。因此,若对玻璃层叠体10施加将支撑基材12和玻璃基板16剥离的方向的应力,则玻璃层叠体10在有机硅树脂层14与玻璃基板16之间剥离,分离为玻璃基板16和带有机硅树脂层的支撑基材18。
剥离强度(x)优选与剥离强度(y)相比足够高。
为了提高有机硅树脂层14对支撑基材12的附着力,优选使后述的固化性有机硅在支撑基材12上固化而形成有机硅树脂层14。利用固化时的粘接力,能够形成以高的结合力与支撑基材12结合的有机硅树脂层14。
另一方面,通常,固化后的有机硅树脂对玻璃基板16的结合力低于在上述固化时产生的结合力。因此,通过在支撑基材12上形成有机硅树脂层14,然后在有机硅树脂层14的面上层叠玻璃基板16,从而能够制造玻璃层叠体10。
以下,首先,对构成玻璃层叠体10的各层(支撑基材12、玻璃基板16、有机硅树脂层14)进行详细叙述,然后,对玻璃层叠体的制造方法进行详细叙述。
<支撑基材>
支撑基材12为支撑并加强玻璃基板16的构件。
作为支撑基材12,例如可以使用玻璃板、塑料板、金属板(例如,SUS板)等。通常,支撑基材12优选由与玻璃基板16的线膨胀系数的差小的材料形成,更优选由与玻璃基板16相同的材料形成。特别优选支撑基材12为由与玻璃基板16相同的玻璃材料形成的玻璃板。
对于支撑基材12的厚度,可以比玻璃基板16厚或薄。从玻璃层叠体10的处理性的方面出发,优选支撑基材12的厚度比玻璃基板16厚。
支撑基材12为玻璃板的情况下,从容易处理、不易破裂等理由出发,玻璃板的厚度优选为0.03mm以上。另外,从期望在剥离玻璃基板时适度地弯曲而不会破裂的刚性的理由出发,玻璃板的厚度优选为1.0mm以下。
支撑基材12与玻璃基板16在25~300℃下的平均线膨胀系数的差优选10×10-7/℃以下、更优选3×10-7/℃以下、进一步优选1×10-7/℃以下。
<玻璃基板>
对玻璃基板16的玻璃的种类没有特别限制,优选无碱硼硅酸盐玻璃、硼硅酸盐玻璃、钠钙玻璃、高二氧化硅玻璃、以及其它的以氧化硅为主要成分的氧化物系玻璃。作为氧化物系玻璃,优选基于氧化物换算得到的氧化硅的含量为40~90质量%的玻璃。
作为玻璃基板16,更具体而言,作为LCD、OLED这样的显示装置用的玻璃基板、电磁波、X射线、紫外线、可见光线、红外线等的接收传感器面板用的玻璃基板,可列举出由无碱硼硅酸盐玻璃形成的玻璃板(旭硝子株式会社制商品名“AN100”)。
对于玻璃基板16的厚度,从薄型化和/或轻量化的观点出发,优选0.5mm以下、更优选0.4mm以下、进一步优选0.2mm以下、特别优选0.10mm以下。0.5mm以下的情况下,能对玻璃基板16赋予良好的柔性。0.2mm以下的情况下,能将玻璃基板16卷取成卷状。
另外,从玻璃基板16的处理容易的方面出发,玻璃基板16的厚度优选0.03mm以上。
进而,对玻璃基板16的面积(主面的面积)没有特别限制,优选为300cm2以上。
需要说明的是,玻璃基板16可以包含2层以上,该情况下,形成各个层的材料可以为同种材料,也可以为不同种材料。另外,该情况下,“玻璃基板16的厚度”是指所有层的合计的厚度。
对玻璃基板16的制造方法没有特别限制,通常,可以将玻璃原料熔融,使熔融玻璃形成板状而获得。这样的成形方法可以为通常的方法,例如可列举出浮法、熔融法、狭缝下拉法等。
<有机硅树脂层>
有机硅树脂层14防止玻璃基板16的位置偏移,并且防止玻璃基板16因分离操作而破损。有机硅树脂层14的和玻璃基板16接触的表面14a与玻璃基板16的第1主面16a密合。
认为有机硅树脂层14与玻璃基板16通过弱的粘接力、起因于范德华力的结合力进行结合。
另外,有机硅树脂层14通过强的结合力与支撑基材12表面结合,作为提高两者的密合性的方法,可以采用公知的方法。例如,如后所述,通过在支撑基材12表面上形成有机硅树脂层14(更具体而言,使可形成规定的有机硅树脂的固化性有机硅(有机聚硅氧烷)在支撑基材12上固化),从而使有机硅树脂层14中的有机硅树脂粘接于支撑基材12表面,能够得到高的结合力。另外,实施使支撑基材12表面与有机硅树脂层14之间产生强的结合力的处理(例如,使用偶联剂的处理),能够提高支撑基材12表面与有机硅树脂层14之间的结合力。
对有机硅树脂层14的厚度没有特别限制,优选100μm以下、更优选50μm以下、进一步优选10μm以下。对下限没有特别限制,大多为0.001μm以上。有机硅树脂层14的厚度为这样的范围时,不易在有机硅树脂层14上产生裂纹,即使在有机硅树脂层14与玻璃基板16之间夹杂气泡、异物,也能够抑制玻璃基板16的变形缺陷的产生。
上述厚度意指平均厚度,为用接触式膜厚测定装置测定5处以上的任意位置的有机硅树脂层14的厚度并对它们进行算术平均而得到的值。
对有机硅树脂层14的玻璃基板16侧的表面的表面粗糙度Ra没有特别限制,从玻璃基板16的层叠性及剥离性更优异的方面出发,优选0.1~20nm、更优选0.1~10nm。
需要说明的是,作为表面粗糙度Ra的测定方法,根据JIS B 0601-2001进行测定,将针对任意5处以上的位置测定而得到的Ra进行算术平均而得到的值相当于上述表面粗糙度Ra。
有机硅树脂层包含选自由3d过渡金属、4d过渡金属、镧系金属及铋(Bi)组成的组中的至少1种金属元素(以后,也将它们统称为“特定元素”)。通过包含这些特定元素,从而抑制在大气气氛下的高温加热处理时有机硅树脂层的端部变质。其理由的详细情况不明确,但可以认为通过使有机硅树脂层中包含特定元素,从而能抑制有机硅树脂的氧化。
作为3d过渡金属,可列举出周期表第4周期的过渡金属即钪(Sc)~铜(Cu)的金属。具体而言,可列举出钪(Sc)、钛(Ti)、钒(V)、铬(Cr)、锰(Mn)、铁(Fe)、钴(Co)、镍(Ni)、及铜(Cu)。
作为4d过渡金属,可列举出周期表第5周期的过渡金属即钇(Y)~银(Ag)的金属。具体而言,可列举出钇(Y)、锆(Zr)、铌(Nb)、钼(Mo)、锝(Tc)、钌(Ru)、铑(Rh)、钯(Pd)、及银(Ag)。
作为镧系金属,可列举出镧(La)~镥(Lu)的金属。具体而言可列举出镧(La)、铈(Ce)、镨(Pr)、钕(Nd)、钷(Pm)、钐(Sm)、铕(Eu)、钆(Gd)、铽(Tb)、镝(Dy)、钬(Ho)、铒(Er)、铥(Tm)、镱(Yb)、及镥(Lu)。
其中,在进一步抑制有机硅树脂层的端部变质的方面,有机硅树脂层优选包含选自由3d过渡金属、镧系金属及铋(Bi)组成的组中的至少1种金属元素,更优选包含选自由铁、锰、铜、铈、钴、镍、铬及铋组成的组中的至少1种金属元素,进一步优选包含选自由铁、锰、铜、铈、铬、及钴组成的组中的至少1种金属元素,特别优选包含选自由铁、锰、铜、铈及铋组成的组中的至少1种金属元素。
需要说明的是,有机硅树脂层可以包含1种上述特定元素,也可以包含2种以上上述特定元素。
对有机硅树脂层中的特定元素的含量没有特别限制,在进一步抑制有机硅树脂层的端部变质的方面,在有机硅树脂层100质量份中优选为0.001质量份以上、更优选为0.01质量份以上。需要说明的是,对有机硅树脂层中的特定元素的含量的上限值没有特别限制,优选为1.0质量份以下、更优选为0.7质量份以下。
有机硅树脂层包含2种以上特定元素的情况下,优选它们的总含量在上述范围内。
需要说明的是,对于特定元素的含量,根据金属的种类适宜选择最适的含量。
另外,有机硅树脂层包含选自由3d过渡金属、镧系金属及铋(Bi)组成的组中的至少1种金属元素(以后,也将它们统称为“适宜特定元素”)的情况下,对有机硅树脂层中的适宜特定元素的含量没有特别限制,在进一步抑制有机硅树脂层的端部变质的方面,在有机硅树脂层100质量份中优选为0.01质量份以上、更优选为0.03质量份以上。对有机硅树脂层中的适宜特定元素的含量的上限值没有特别限制,优选为0.7质量份以下、更优选为0.5质量份以下。
有机硅树脂层包含2种以上适宜特定元素的情况下,优选它们的总含量在上述范围内。
有机硅树脂层可以包含除上述特定元素以外的其它金属元素(例如,锡元素、铝元素、铂元素)。
另外,有机硅树脂层中可以包含促进缩合反应的固化催化剂、促进加成反应的固化催化剂。作为促进缩合反应的固化催化剂,例如可列举出三乙酰丙酮铝、三(乙基乙酰乙酸基)铝等铝螯合物、二月桂酸二丁基锡、双(2-乙基己酸)锡(II)等锡化合物。作为促进加成反应的固化催化剂,例如可列举出铂系催化剂。
需要说明的是,有机硅树脂层包含锡元素的情况下,层叠于有机硅树脂层上的玻璃基板的剥离强度容易降低,玻璃基板的剥离容易实施。另外,从有机硅树脂层的耐热性及基板的剥离性的平衡的方面出发,优选上述锡元素与锆元素组合使用。即,有机硅树脂层包含锡元素的情况下,优选也包含锆元素。
另外,有机硅树脂层包含铝元素的情况下,有机硅树脂层的耐热性容易提高。
上述特定元素及上述其它金属元素在有机硅树脂层中可以为金属的形态、离子的形态、化合物的形态、及络合物的形态中的任意形态。
有机硅树脂层中的特定元素及上述其它金属元素的测定方法没有特别限制,可以采用公知的方法,例如可列举出ICP发射光谱法(ICP-AES)、或ICP质谱法(ICP-MS)。作为上述方法中使用的装置,可列举出电感耦合型等离子体发射光谱分析装置PS3520UVDDII(Hitachi High-Technologies Corporation.)、电感耦合等离子体(三重四极杆)质谱仪Agilent8800(Agilent technologies公司)。
作为基于上述方法的具体的步骤的一例,首先,测定有机硅树脂层的质量。接着,使用氧燃烧器等,使有机硅树脂层氧化、并进行二氧化硅化。然后,为了从经氧化的有机硅树脂层去除SiO2成分,用氢氟酸对经氧化的有机硅树脂层进行清洗。使得到的残渣溶解于盐酸,用上述ICP发射光谱法(ICP-AES)、或ICP质谱法(ICP-MS)进行规定的特定元素和/或其它金属元素的定量。然后,算出特定元素或其它金属元素相对于预先测定的有机硅树脂层的质量的含量。
对形成包含特定元素的有机硅树脂层的方法没有特别限制,可列举出使用含有后述的固化性有机硅及包含特定元素的金属化合物的固化性组合物来形成有机硅树脂层的方法。
需要说明的是,作为在有机硅树脂层中导入其它金属元素的方法,可列举出与上述特定元素同样地,使用含有后述的固化性有机硅、包含特定元素的金属化合物、及包含其它金属元素的金属化合物的上述固化性组合物来形成有机硅树脂层的方法。
详细的情况在后段中进行详细叙述。
(有机硅树脂)
有机硅树脂层14主要由有机硅树脂形成。
通常,有机甲硅烷氧基单元有被称为M单元的1官能有机甲硅烷氧基单元、被称为D单元的2官能有机甲硅烷氧基单元、被称为T单元的3官能有机甲硅烷氧基单元、及被称为Q单元的4官能有机甲硅烷氧基单元。需要说明的是,Q单元为不具有与硅原子键合的有机基团(具有与硅原子键合的碳原子的有机基团)的单元,但在本发明中视为有机甲硅烷氧基单元(含硅键合单元)。需要说明的是,将形成M单元、D单元、T单元、Q单元的单体分别也称为M单体、D单体、T单体、Q单体。
需要说明的是,全部有机甲硅烷氧基单元意指M单元、D单元、T单元、及Q单元的合计。M单元、D单元、T单元、及Q单元的数量(摩尔量)的比率可以由基于29Si-NMR得到的峰面积比的值来计算。
有机甲硅烷氧基单元中,硅氧烷键为2个硅原子借助1个氧原子键合而成的键,因此将硅氧烷键中的平均1个硅原子的氧原子视为1/2个,式中表示为O1/2。更具体而言,例如,1个D单元中,其1个硅原子与2个氧原子键合,各氧原子与其它单元的硅原子键合,由此其式成为-O1/2-(R)2Si-O1/2-(R表示氢原子或有机基团)。因为存在2个O1/2,所以D单元通常表示为(R)2SiO2/2(换言之,(R)2SiO)。
需要说明的是,以下的说明中,与其它硅原子键合的氧原子O*为将2个硅原子间结合的氧原子,意指Si-O-Si所示的键中的氧原子。因此,在2个有机甲硅烷氧基单元的硅原子间存在1个O*。
M单元意指(R)3SiO1/2所示的有机甲硅烷氧基单元。此处,R表示氢原子或有机基团。(R)后记载的数字(此处为3)意指3个氢原子或有机基团键合于硅原子上。即,M单元具有1个硅原子、3个氢原子或有机基团、和1个氧原子O*。更具体而言,M单元具有:与1个硅原子键合的3个氢原子或有机基团、和与1个硅原子键合的氧原子O*。
D单元意指(R)2SiO2/2(R表示氢原子或有机基团)所示的有机甲硅烷氧基单元。即,D单元为具有1个硅原子、且具有与该硅原子键合的2个氢原子或有机基团、以及2个与其它硅原子键合的氧原子O*的单元。
T单元意指RSiO3/2(R表示氢原子或有机基团)所示的有机甲硅烷氧基单元。即,T单元为具有1个硅原子、且具有与该硅原子键合的1个氢原子或有机基团、和3个与其它硅原子键合的氧原子O*的单元。
Q单元意指SiO2所示的有机甲硅烷氧基单元。即,Q单元为具有1个硅原子、且具有4个与其它硅原子键合的氧原子O*的单元。
需要说明的是,作为有机基团,例如可列举出甲基、乙基、丙基、丁基、戊基、己基、环己基、庚基等烷基;苯基、甲苯基、二甲苯基、萘基等芳基;苄基、苯乙基等芳烷基;卤化烷基(例如,氯甲基、3-氯丙基、3,3,3-三氟丙基等)等卤素取代的一价烃基。需要说明的是,作为有机基团,优选碳数1~12(优选碳数1~10左右)的、无取代或卤素取代的一价烃基。
对于构成有机硅树脂层14的有机硅树脂,其结构没有特别限制,在玻璃基板16的层叠性及剥离性的平衡更优异的方面,优选包含选自由(R)3SiO1/2所示的有机甲硅烷氧基单元(M单元)及(R)SiO3/2所示的有机甲硅烷氧基单元(T单元)组成的组中的至少1种特定有机甲硅烷氧基单元。
另外,对于上述特定有机甲硅烷氧基单元的比率,相对于全部有机甲硅烷氧基单元,优选为60摩尔%以上、更优选为80摩尔%以上。对上限没有特别限制,大多为100摩尔%以下。需要说明的是,M单元、T单元的数量(摩尔量)的比率可以由基于29Si-NMR得到的峰面积比的值来计算。
有机硅树脂通常可以将通过固化处理可形成该有机硅树脂的固化性有机硅固化(交联固化)来获得。即,有机硅树脂相当于固化性有机硅的固化物。
固化性有机硅根据其固化机制分类为缩合反应型有机硅、加成反应型有机硅、紫外线固化型有机硅及电子射线固化型有机硅,均可以使用。其中,优选缩合反应型有机硅及加成反应型有机硅。
作为缩合反应型有机硅,可以适当地使用作为单体的水解性有机硅烷化合物或其混合物(单体混合物)、或者使单体或单体混合物进行部分水解缩合反应而得到的部分水解缩合物(有机聚硅氧烷)。另外,也可以为部分水解缩合物与单体的混合物。需要说明的是,单体可以单独使用1种、也可以组合使用2种以上。通过使用该缩合反应型有机硅,进行水解·缩合反应(溶胶凝胶反应),从而能够形成有机硅树脂。
上述单体(水解性有机硅烷化合物)通常由(R’-)aSi(-Z)4-a表示。其中,a表示0~3的整数、R’表示氢原子或有机基团、Z表示羟基或水解性基团。该化学式中,a=3的化合物为M单体、a=2的化合物为D单体、a=1的化合物为T单体、a=0的化合物为Q单体。单体中,通常,Z基为水解性基团。另外,存在2个或3个R’的情况下(a为2个或3个的情况下),多个R’可以不同。
作为部分水解缩合物的固化性有机硅可通过将单体的Z基的一部分转化为氧原子O*的反应来获得。单体的Z基为水解性基团的情况下,Z基通过水解反应转化为羟基,接着通过键合于其它硅原子的2个羟基之间的脱水缩合反应,2个硅原子借助氧原子O*键合。羟基(或未水解的Z基)残留于固化性有机硅中,在固化性有机硅的固化时,这些羟基、Z基与上述同样地反应而固化。固化性有机硅的固化物通常形成三维交联而成的聚合物(有机硅树脂)。
单体的Z基为水解性基团的情况下,作为该Z基,可列举出烷氧基、卤素原子(例如,氯原子)、酰氧基、异氰酸酯基等。大多情况下,作为单体,使用Z基为烷氧基的单体,这样的单体也称为烷氧基硅烷。
烷氧基与氯原子等其它水解性基团相比为反应性较低的水解性基团,在使用Z基为烷氧基的单体(烷氧基硅烷)得到的固化性有机硅中,往往与羟基一起存在未反应的烷氧基作为Z基。
作为上述缩合反应型有机硅,从反应的控制、处理的方面出发,优选由水解性有机硅烷化合物得到的部分水解缩合物(有机聚硅氧烷)。部分水解缩合物是使水解性有机硅烷化合物发生部分水解缩合而得到的。对部分水解缩合的方法没有特别限制。通常使水解性有机硅烷化合物在溶剂中、在催化剂存在下反应来制造。作为催化剂,可列举出酸催化剂及碱催化剂。另外,水解反应中通常优选使用水。作为部分水解缩合物,优选在溶剂中使水解性有机硅烷化合物在酸或碱水溶液的存在下反应而制造的物质。
作为使用的水解性有机硅烷化合物的适宜形态,如上所述可列举出烷氧基硅烷。即,作为固化性有机硅的适宜形态之一,可列举出通过烷氧基硅烷的水解反应及缩合反应得到的固化性有机硅。
使用烷氧基硅烷的情况下,部分水解缩合物的聚合度容易变大,本发明的效果更优异。
作为加成反应型有机硅,可以适当地使用包含主剂及交联剂、在铂催化剂等催化剂的存在下进行固化的固化性的组合物。通过加热处理,可促进加成反应型有机硅的固化。加成反应型有机硅中的主剂优选为具有与硅原子键合的烯基(乙烯基等)的有机聚硅氧烷(即有机烯基聚硅氧烷。需要说明的是,优选直链状),烯基等成为交联点。加成反应型有机硅中的交联剂优选为具有与硅原子键合的氢原子(氢化甲硅烷基)的有机聚硅氧烷(即有机氢聚硅氧烷。需要说明的是,优选直链状),氢化甲硅烷基等成为交联点。
加成反应型有机硅通过主剂与交联剂的交联点发生加成反应而固化。需要说明的是,在源自交联结构的耐热性更优异的方面,有机氢聚硅氧烷的与硅原子键合的氢原子相对于有机烯基聚硅氧烷的烯基的摩尔比优选为0.5~2。
对上述缩合反应型有机硅及加成反应型有机硅等固化性有机硅的重均分子量(Mw)没有特别限制,优选5000~60000、更优选5000~30000。若Mw为5000以上,则在涂布性的观点上优异,若Mw为60000以下,则在溶剂中的溶解性、涂布性的观点上优异。
对上述有机硅树脂层14的制造方法没有特别限制,可以采用公知的方法。其中,在有机硅树脂层14的生产率优异的方面,作为有机硅树脂层14的制造方法,优选在支撑基材12上涂布含有形成上述有机硅树脂的固化性有机硅及包含特定元素的金属化合物的固化性组合物,根据需要去除溶剂,形成涂膜,使涂膜中的固化性有机硅固化,从而制成有机硅树脂层14。
如上所述,作为固化性有机硅,可以使用作为单体的水解性有机硅烷化合物、和/或使单体进行部分水解缩合反应而得到的部分水解缩合物(有机聚硅氧烷)。另外,作为固化性有机硅,也可以使用有机烯基聚硅氧烷及有机氢聚硅氧烷的混合物。
上述固化性组合物中所含的包含特定元素的金属化合物只要包含规定的特定元素,就对其结构没有特别限制,可列举出公知的金属化合物。需要说明的是,本说明书中,所谓的络合物包含在上述金属化合物中。
作为包含特定元素的金属化合物,优选包含特定元素的络合物。络合物是指以金属元素的原子或离子为中心,并使配体(原子、原子团、分子或离子)与其键合而成的集合体。
对上述络合物中所含的配体的种类没有特别限制,例如可列举出选自由β-二酮、羧酸、醇盐及醇组成的组中的配体。
作为β-二酮,例如可列举出乙酰丙酮、乙酰乙酸甲酯、乙酰乙酸乙酯、苯甲酰丙酮等。
作为羧酸,例如可列举出乙酸、2-乙基己酸、环烷酸、新癸酸等。
作为醇盐,例如可列举出甲醇盐、乙醇盐、异丙醇盐、丁醇盐等。
作为醇,例如可列举出甲醇、乙醇、正丙醇、异丙醇、正丁醇、叔丁醇等。
作为上述包含特定元素的金属化合物,具体而言,可列举出三(2,4-戊二酮酸)锰(III)等有机锰化合物、三(2,4-戊二酮酸)铁(III)、三(2-乙基己酸)铁(III)等有机铁化合物、双(2,4-戊二酮酸)钴(II)等有机钴化合物、双(2,4-戊二酮酸)镍(II)等有机镍化合物、新癸酸铜(II)等有机铜化合物、新癸酸铋(III)等有机铋化合物、四(单甲基乙醇)锆、四(单乙基乙醇)锆、四(单丁基乙醇)锆、正丙醇锆等有机锆化合物、三(2-乙基己酸)铈(III)等有机铈化合物、三(2,4-戊二酮酸)铬(III)等有机铬化合物。
对固化性组合物中的包含特定元素的金属化合物的含量没有特别限制,优选以上述有机硅树脂层中的特定元素的含量为适当范围的方式进行调整。
使用缩合反应型有机硅作为固化性有机硅的情况下,根据需要,固化性组合物可以包含促进缩合反应的固化催化剂作为包含其它金属元素的金属化合物。作为促进缩合反应的固化催化剂,例如可列举出三乙酰丙酮铝、三(乙基乙酰乙酸基)铝等铝螯合物、二月桂酸二丁基锡、双(2-乙基己酸)锡(II)等锡化合物。
使用加成反应型有机硅作为固化性有机硅的情况下,根据需要,固化性组合物可以包含铂催化剂作为包含其它金属元素的金属化合物。
铂催化剂为用于使上述有机烯基聚硅氧烷中的烯基与上述有机氢聚硅氧烷中的氢原子的氢化硅烷化反应进行·促进的催化剂。
固化性组合物中可以包含溶剂,该情况下,通过调整溶剂的浓度,能够控制涂膜的厚度。其中,从处理性优异、有机硅树脂层14的膜厚的控制更容易的方面出发,含有固化性有机硅的固化性组合物中的固化性有机硅的含量相对于组合物全部质量,优选1~80质量%、更优选1~50质量%。
作为溶剂,只要为在作业环境下能够容易溶解固化性有机硅、并且能够容易挥发去除的溶剂,就没有特别限制。具体而言,例如可列举出乙酸丁酯、2-庚酮、1-甲氧基-2-丙醇乙酸酯、八甲基环四硅氧烷、异构烷烃系溶剂等。
另外,固化性组合物中可以包含各种添加剂。例如,可以包含流平剂。作为流平剂,可列举出Megafac F558、Megafac F560、Megafac F561(均为DIC株式会社制)等氟系的流平剂。
<玻璃层叠体及其制造方法>
玻璃层叠体10如上所述为包含支撑基材12及玻璃基板16、以及配置于它们之间的有机硅树脂层14的层叠体。
对玻璃层叠体10的制造方法没有特别限制,为了得到剥离强度(x)高于剥离强度(y)的层叠体,优选在支撑基材12表面上形成有机硅树脂层14的方法。其中,优选如下方法:在支撑基材12的表面涂布含有固化性有机硅及包含特定元素的金属化合物的固化性组合物,对得到的涂膜实施固化处理从而得到有机硅树脂层14后,接着在有机硅树脂层14的表面层叠玻璃基板16,制造玻璃层叠体10的方法。
可以认为,若使固化性有机硅在支撑基材12表面固化,则通过固化反应时的与支撑基材12表面的相互作用而粘接,有机硅树脂与支撑基材12表面的剥离强度变高。因此,即使玻璃基板16与支撑基材12由相同材质形成,也能够对有机硅树脂层14与两者间的剥离强度设计差异。
以下,将在支撑基材12的表面形成固化性有机硅的层、并在支撑基材12表面上形成有机硅树脂层14的工序称为树脂层形成工序1,将在有机硅树脂层14的表面层叠玻璃基板16而制成玻璃层叠体10的工序称为层叠工序1,对各工序的步骤进行详细叙述。
(树脂层形成工序1)
树脂层形成工序1中,在支撑基材12的表面形成固化性有机硅的层,在支撑基材12表面上形成有机硅树脂层14。
首先,为了在支撑基材12上形成固化性有机硅的层,在支撑基材12上涂布上述固化性组合物。接着,优选对固化性有机硅的层实施固化处理,从而形成固化层。
对在支撑基材12表面上涂布固化性组合物的方法没有特别限制,可列举出公知的方法。例如,可列举出喷涂法、模涂法、旋转涂布法、浸渍涂布法、辊涂法、棒涂法、丝网印刷法、凹版涂布法等。
接着,使支撑基材12上的固化性有机硅固化,形成固化层(有机硅树脂层)。
对固化的方法没有特别限制,可以根据使用的固化性有机硅的种类适宜实施最适的处理。例如,使用缩合反应型有机硅及加成反应型有机硅的情况下,作为固化处理,优选热固化处理。
热固化的温度条件优选150~550℃、更优选200~450℃。另外,加热时间通常优选10~300分钟、更优选20~120分钟。需要说明的是,对于加热条件,可以改变温度条件而分阶段实施。
需要说明的是,热固化处理中,优选进行实施了预固化(预备固化)的后固化(正式固化)。通过进行预固化,从而得到耐热性优异的有机硅树脂层14。
(层叠工序1)
层叠工序1为在上述的树脂层形成工序中得到的有机硅树脂层14的表面上层叠玻璃基板16,得到依次具备支撑基材12、有机硅树脂层14和玻璃基板16的玻璃层叠体10的工序。
对在有机硅树脂层14上层叠玻璃基板16的方法没有特别限制,可列举出公知的方法。
例如,可列举出在常压环境下在有机硅树脂层14的表面上层叠玻璃基板16的方法。需要说明的是,根据需要,在有机硅树脂层14的表面上层叠玻璃基板16后,也可以使用辊、压制机将玻璃基板16压接于有机硅树脂层14。通过利用辊或压制机进行压接,混入至有机硅树脂层14与玻璃基板16之间的气泡较容易被去除,故优选。
若通过真空层压法、真空压制法进行压接,则可抑制气泡的混入,并且能够实现良好的密合,是优选的。通过在真空下进行压接,还存在如下优点:即使在残留有微小的气泡的情况下,气泡也不会因加热而成长、不易引起玻璃基板16的变形缺陷。
优选在层叠玻璃基板16时对与有机硅树脂层14接触的玻璃基板16的表面进行充分清洗,在清洁度高的环境下进行层叠。清洁度越高,玻璃基板16的平坦性越好,故优选。
需要说明的是,层叠玻璃基板16后,根据需要可以进行预退火处理(加热处理)。通过进行该预退火处理,从而层叠的玻璃基板16对有机硅树脂层14的密合性提高,能够实现适当的剥离强度(y)。
需要说明的是,上述中,对使用玻璃基板作为基板的情况进行了详细叙述,但对基板的种类没有特别限制。
例如,作为基板,可列举出金属基板、半导体基板、树脂基板及玻璃基板。另外,基板例如可以如由2种不同的金属构成的金属板那样,为由多个同种材料构成的基板。进而,基板例如可以如由树脂和玻璃构成的基板那样,为不同种材料(例如选自金属、半导体、树脂及玻璃的2种以上的材料)的复合体基板。
对金属板、半导体基板等基板的厚度没有特别限制,从薄型化和/或轻量化的观点出发,优选为0.5mm以下、更优选为0.4mm以下、进一步优选为0.2mm以下。另外,对厚度的下限没有特别限制,优选为0.005mm以上。
另外,对基板的面积(主面的面积)没有特别限制,从电子器件的生产率的方面出发,优选为300cm2以上。
另外,对基板的形状没有特别限制,可以为矩形状,也可以为圆形状。另外,基板上可以形成有定向平面(在基板的外周形成的平坦部分)、切口(在基板的外周缘形成的一个或一个以上的V型缺口)。
<树脂基板及使用了树脂基板的层叠体的制造方法>
作为上述树脂基板,优选使用能耐受器件的制造工序中的热处理的耐热性优异的树脂基板。作为构成树脂基板的树脂,例如可列举出聚苯并咪唑树脂(PBI)、聚酰亚胺树脂(PI)、聚醚醚酮树脂(PEEK)、聚酰胺树脂(PA)、氟树脂、环氧树脂、聚苯硫醚树脂(PPS)等。特别是,从优异的耐热性、优异的耐化学药品性、低热膨胀系数、高机械特性等的观点出发,优选由聚酰亚胺树脂形成的聚酰亚胺树脂基板。
另外,为了在树脂基板上形成电子器件的高精细的布线等,优选树脂基板的表面平滑。具体而言,树脂基板的表面粗糙度Ra优选50nm以下、更优选30nm以下、进一步优选10nm以下。
对于树脂基板的厚度,从在制造工序中的处理性的观点出发,优选1μm以上、更优选10μm以上。另外,从柔软性的观点出发,优选1mm以下、更优选0.2mm以下。
对于树脂基板的热膨胀系数,与电子器件、支撑基材的热膨胀系数差小者由于能够抑制加热后或冷却后的层叠体的翘曲,因此优选。具体而言,树脂基板与支撑基材的热膨胀系数之差优选0~90×10-6/℃、更优选0~30×10-6/℃。
对使用树脂基板作为基板时的层叠体的制造方法没有特别限制,例如,可以通过与上述的使用了玻璃基板的情况同样的方法制造层叠体。即,可以在支撑基材上形成有机硅树脂层,在有机硅树脂层上层叠树脂基板,从而制造层叠体。
需要说明的是,以后将依次具备支撑基材、有机硅树脂层和树脂基板的层叠体也称为树脂层叠体。
另外,作为树脂层叠体的其它制造方法,也优选在树脂基板表面上形成有机硅树脂层,制造树脂层叠体的方法。
有机硅树脂层对树脂基板的密合性通常存在较低的倾向。因此,在树脂基板表面上形成有机硅树脂层、并将得到的带有机硅树脂层的树脂基板和支撑基材层叠而得到树脂层叠体的情况下,也有支撑基材与有机硅树脂层之间的剥离强度(x)高于有机硅树脂层与树脂基板之间的剥离强度(y′)的倾向。特别是,使用玻璃板作为支撑基材的情况下,该倾向强。
即,树脂层叠体与玻璃层叠体的情况同样地,能分离为树脂基板和带有机硅树脂层的支撑基材。
上述树脂层叠体的其它制造方法主要具有:在树脂基板的表面形成固化性有机硅的层,在树脂基板表面上形成有机硅树脂层的工序(树脂层形成工序2);及在有机硅树脂层的表面层叠支撑基材而制成树脂层叠体的工序(层叠工序2)。
以下,对上述各工序的步骤进行详细叙述。
(树脂层形成工序2)
树脂层形成工序2为在树脂基板的表面形成固化性有机硅的层、在树脂基板表面上形成有机硅树脂层的工序。通过本工序,可得到依次具备树脂基板和有机硅树脂层的带有机硅树脂层的树脂基板。
本工序中,为了在树脂基板上形成固化性有机硅的层,在树脂基板上涂布上述固化性组合物。接着,优选对固化性有机硅的层实施固化处理,从而形成固化层。
对在树脂基板表面上涂布固化性组合物的方法没有特别限制,可列举出公知的方法。例如,可列举出喷涂法、模涂法、旋转涂布法、浸渍涂布法、辊涂法、棒涂法、丝网印刷法、凹版涂布法等。
接着,使树脂基板上的固化性有机硅固化,形成固化层(有机硅树脂层)。
对固化的方法没有特别限制,可以根据使用的固化性有机硅的种类适宜实施最适的处理。例如,使用缩合反应型有机硅及加成反应型有机硅的情况下,作为固化处理,优选热固化处理。
对于热固化处理的条件,在树脂基板的耐热性的范围内实施,例如,热固化的温度条件优选50~400℃、更优选100~300℃。另外,加热时间通常优选10~300分钟、更优选20~120分钟。
形成的有机硅树脂层的方案如上所述。
(层叠工序2)
层叠工序2为在有机硅树脂层的表面上层叠支撑基材而制成树脂层叠体的工序。即,本工序为使用带有机硅树脂层的树脂基板和支撑基材来形成树脂层叠体的工序。
对将支撑基材层叠于有机硅树脂层上的方法没有特别限制,可列举出公知的方法,可列举出上述玻璃层叠体的制造中的层叠工序1的说明中举出的方法。
需要说明的是,层叠支撑基材后,可以根据需要进行加热处理。通过进行加热处理,从而层叠的支撑基材对有机硅树脂层的密合性提高,能够实现适当的剥离强度(x)。
加热处理的温度条件优选50~400℃、更优选100~300℃。另外,加热时间通常优选1~120分钟、更优选5~60分钟。需要说明的是,加热条件可以改变温度条件而分阶段地实施。
另外,在后述的形成电子器件用构件的工序中加热树脂层叠体的情况下,可以省略加热处理。
从提高剥离强度(x)、调节剥离强度(x)与剥离强度(y’)的平衡的观点出发,优选在将支撑基材层叠于有机硅树脂层上之前对支撑基材及有机硅树脂层中的至少一者实施表面处理,更优选对有机硅树脂层实施表面处理。
作为表面处理的方法,例如可列举出电晕处理、等离子体处理、UV臭氧处理等,其中,优选电晕处理。
带有机硅树脂层的树脂基板能通过在卷成卷状的树脂基板的表面上形成有机硅树脂层后再次卷取成卷状的所谓卷对卷(Roll to Roll)方式制造,生产效率优异。
在支撑基材上形成有机硅树脂层的情况下,在支撑基材上涂布固化性组合物时,由于所谓咖啡环现象,存在有机硅树脂层的外周部的厚度与中央部的厚度相比变厚的倾向。该情况下,需要将配置有有机硅树脂层的外周部的支撑基材部分切断而去除,在支撑基材为玻璃板的情况下,其花费的工夫和成本大。
另一方面,在树脂基板上形成有机硅树脂层的情况下,通常树脂基板的处理性、成本优异,因此即使产生了如上所述的问题,配置有有机硅树脂层的外周部的树脂基板部分的切除也比较容易。
<半导体基板及使用了半导体基板的层叠体的制造方法>
作为上述半导体基板的材料,可列举出Si、SiC、GaN、氧化镓、金刚石等。将Si的基板也称为Si晶圆。
为了在半导体基板上形成电子器件的高精细的布线等,半导体基板的表面优选平滑。具体而言,半导体基板的表面粗糙度Ra优选50nm以下、更优选30nm以下、进一步优选10nm以下。
对于半导体基板的厚度,从制造工序中的处理性的观点出发,优选1μm以上、更优选10μm以上。从电子器件的小型化的观点出发,优选1mm以下、更优选0.2mm以下。
对于半导体基板的热膨胀系数,与电子器件、支撑基材的热膨胀系数差小者由于能够抑制加热后或冷却后的层叠体的翘曲,因此优选。具体而言,半导体基板与支撑基材的热膨胀系数之差优选0~90×10-6/℃、更优选0~30×10-6/℃。
对使用半导体基板作为基板时的层叠体的制造方法没有特别限制,例如,可以通过与上述的使用了玻璃基板的情况同样的方法制造层叠体。即,可以在支撑基材上形成有机硅树脂层,在有机硅树脂层上层叠半导体基板,从而制造层叠体。
以后将依次具备支撑基材、有机硅树脂层和半导体基板的层叠体也称为半导体层叠体。
需要说明的是,如后述那样,在半导体层叠体中也抑制了端部变质。
(层叠体)
本发明的层叠体(例如,上述的玻璃层叠体10)可以用于各种用途,例如,可列举出制造后述的显示装置用面板、PV、薄膜二次电池、表面形成有电路的半导体晶圆、接收传感器面板等电子部件的用途。需要说明的是,该用途中,也存在层叠体在大气气氛下、高温条件下(例如,450℃以上)暴露(例如,20分钟以上)的情况。
此处,显示装置用面板包含LCD、OLED、电子纸、等离子体显示器面板、场发射面板、量子点LED面板、微型LED显示器面板、MEMS(微型机电系统,Micro Electro MechanicalSystems)快门面板等。
此处,接收传感器面板包含电磁波接收传感器面板、X射线光接收传感器面板、紫外线光接收传感器面板、可见光光接收传感器面板、红外线光接收传感器面板等。这些接收传感器面板中使用的基板可以用树脂等加强片进行了加强。
需要说明的是,图1中示出了1个基板(例如,玻璃基板、树脂基板或半导体基板)夹着有机硅树脂层层叠于支撑基材的方案。但是,本发明的层叠体不限定于该方案,例如,也可以为多个基板夹着有机硅树脂层层叠于支撑基材的方案(以下,也称为“多面粘贴方案”)。
多面粘贴方案更详细而言为多个基板均夹着有机硅树脂层与支撑基材接触的方案。即,不是多张基板重叠的(仅多张中的1张基板夹着有机硅树脂层与支撑基材接触的)方案。
多面粘贴方案中,例如,可以在各个基板的每个上设置多个有机硅树脂层,在1个支撑基材上配置多个基板及有机硅树脂层。然而不限定于此,例如,可以在形成于1个支撑基材上的1张有机硅树脂层(例如,与支撑基材相同尺寸)上配置各个基板。
<电子器件及其制造方法>
本发明中,使用上述的层叠体,制造包含基板、电子器件用构件的电子器件(以后,也适宜地称为“带构件的基板”)。
以下,对使用了上述玻璃层叠体10的电子器件的制造方法进行详细叙述。
对电子器件的制造方法没有特别限制,从电子器件的生产率优异的方面出发,优选如下方法:在上述玻璃层叠体中的玻璃基板上形成电子器件用构件,制造带电子器件用构件的层叠体,从得到的带电子器件用构件的层叠体以有机硅树脂层的玻璃基板侧界面作为剥离面而分离为电子器件(带构件的基板)和带有机硅树脂层的支撑基材的方法。
以下,将在上述玻璃层叠体中的玻璃基板上形成电子器件用构件,制造带电子器件用构件的层叠体的工序称为构件形成工序;将从带电子器件用构件的层叠体以有机硅树脂层的玻璃基板侧界面作为剥离面而分离为带构件的基板和带有机硅树脂层的支撑基材的工序称为分离工序。
以下,对各工序中使用的材料及步骤进行详细叙述。
(构件形成工序)
构件形成工序为在上述玻璃层叠体10中的玻璃基板16上形成电子器件用构件的工序。更具体而言,如图2的(A)所示,在玻璃基板16的第2主面16b(露出表面)上形成电子器件用构件20,得到带电子器件用构件的层叠体22。
首先,对本工序中使用的电子器件用构件20进行详细叙述,其后对工序的步骤进行详细叙述。
(电子器件用构件(功能性元件))
电子器件用构件20为形成在玻璃层叠体10中的玻璃基板16上的、构成电子器件的至少一部分的构件。更具体而言,作为电子器件用构件20,可列举出显示装置用面板、太阳能电池、薄膜二次电池、或表面形成有电路的半导体晶圆等电子部件、接收传感器面板等中所使用的构件(例如,显示装置用构件、太阳能电池用构件、薄膜二次电池用构件、电子部件用电路、接收传感器用构件)。
例如,作为太阳能电池用构件,对于硅型,可列举出正极的氧化锡等透明电极、以p层/i层/n层为代表的硅层、及负极的金属等,此外,可列举出与化合物型、色素敏化型、量子点型等对应的各种构件等。
另外,作为薄膜二次电池用构件,对于锂离子型,可列举出正极及负极的金属或金属氧化物等透明电极、电解质层的锂化合物、集电层的金属、作为密封层的树脂等,此外,可列举出与镍氢型、聚合物型、陶瓷电解质型等对应的各种构件等。
另外,作为电子部件用电路,CCD、CMOS中,可列举出导电部的金属、绝缘部的氧化硅、氮化硅等,此外,可列举出与压力传感器/加速度传感器等各种传感器、刚性印刷电路板、柔性印刷电路板、刚性柔性印刷电路板等相对应的各种构件等。
(工序的步骤)
对上述带电子器件用构件的层叠体22的制造方法没有特别限制,根据电子器件用构件的构成构件的种类,通过以往公知的方法,在玻璃层叠体10的玻璃基板16的第2主面16b上形成电子器件用构件20。
需要说明的是,电子器件用构件20可以不是在玻璃基板16的第2主面16b上最终形成的构件的全部(以下,称为“全部构件”),而是全部构件的一部分(以下,称为“部分构件”)。也可以将从有机硅树脂层14剥离的带部分构件的基板在之后的工序中作为带全部构件的基板(相当于后述的电子器件)。
另外,对于从有机硅树脂层14剥离的带全部构件的基板,可以在其剥离面(第1主面16a)上形成有其它电子器件用构件。进而,也可以使用2张带全部构件的层叠体进行组装,然后,从带全部构件的层叠体将2张带有机硅树脂层的支撑基材剥离,制造具有2张玻璃基板的带构件的基板。
例如,以制造OLED的情况为例,为了在玻璃层叠体10的玻璃基板16的与有机硅树脂层14侧处于相反侧的表面上(相当于玻璃基板16的第2主面16b)形成有机EL结构体,可以进行形成透明电极、进而在形成有透明电极的面上蒸镀空穴注入层/空穴输送层/发光层/电子输送层等、形成背面电极、使用密封板进行密封等各种层形成、处理。作为这些层形成、处理,具体而言,例如可列举出成膜处理、蒸镀处理、密封板的粘接处理等。
另外,例如,制造TFT-LCD的情况下,具有如下工序等各种工序:TFT形成工序,在玻璃层叠体10的玻璃基板16的第2主面16b上,使用抗蚀液,对通过CVD法及溅射法等通常的成膜法形成的金属膜及金属氧化膜等进行图案形成,形成薄膜晶体管(TFT);CF形成工序,在另一玻璃层叠体10的玻璃基板16的第2主面16b上,将抗蚀液用于图案形成而形成滤色器(CF);以及贴合工序,将TFT形成工序中得到的带TFT的层叠体和CF形成工序中得到的带CF的层叠体层叠。
例如,制造微型LED显示器的情况下,具有:TFT形成工序,至少在玻璃层叠体10的玻璃基板16的第2主面16b上,使用抗蚀液,对通过CVD法及溅射法等通常的成膜法形成的金属膜及金属氧化膜等进行图案形成,形成薄膜晶体管(TFT);及LED安装工序,在形成的TFT上安装LED芯片。另外,除此以外还可以实施平坦化、布线形成、密封等工序。
在TFT形成工序、CF形成工序中,使用周知的光刻技术、蚀刻技术等,在玻璃基板16的第2主面16b形成TFT、CF。此时,作为图案形成用的涂布液,可以使用抗蚀液。
需要说明的是,在形成TFT、CF前,可以根据需要对玻璃基板16的第2主面16b进行清洗。作为清洗方法,可以使用周知的干法清洗、湿法清洗。
贴合工序中,使带TFT的层叠体的薄膜晶体管形成面与带CF的层叠体的滤色器形成面相对,使用密封剂(例如,单元形成用紫外线固化型密封剂)使之贴合。然后,向由带TFT的层叠体和带CF的层叠体形成的单元内注入液晶材料。作为注入液晶材料的方法,例如有减压注入法、滴加注入法。
需要说明的是,在制造电子器件用构件20时,可以包括在大气气氛下、在450℃以上进行加热的条件。为本发明的层叠体时,即使在上述条件下也可抑制有机硅树脂层的端部变质。
(分离工序)
分离工序如图2的(B)所示为如下工序:从上述构件形成工序中得到的带电子器件用构件的层叠体22,将有机硅树脂层14与玻璃基板16的界面作为剥离面,分离为层叠有电子器件用构件20的玻璃基板16(带构件的基板)、和带有机硅树脂层的支撑基材18,得到包含电子器件用构件20及玻璃基板16的带构件的基板(电子器件)24的工序。
剥离时的玻璃基板16上的电子器件用构件20为必需的全部构成构件的形成的一部分的情况下,分离后也可以在玻璃基板16上形成剩余的构成构件。
对剥离玻璃基板16和有机硅树脂层14的方法没有特别限制。例如,可以在玻璃基板16与有机硅树脂层14的界面插入锐利的刀具状物,赋予剥离起点后,吹送水与压缩空气的混合流体而进行剥离。优选的是,以带电子器件用构件的层叠体22的支撑基材12为上侧、电子器件用构件20侧为下侧的方式设置在平板上,使电子器件用构件20侧真空吸附于平板上,在该状态下首先使刀具侵入至玻璃基板16-有机硅树脂层14界面。而且,其后以多个真空吸附垫吸附支撑基材12侧,并从插入了刀具的部位附近依次使真空吸附垫上升。由此,向有机硅树脂层14与玻璃基板16的界面、有机硅树脂层14的内聚破坏面形成空气层,且该空气层在界面、内聚破坏面的整面扩散,能够容易地将带有机硅树脂层的支撑基材18剥离。
另外,带有机硅树脂层的支撑基材18可以与新的玻璃基板层叠,制造本发明的玻璃层叠体10。
需要说明的是,在从带电子器件用构件的层叠体22分离带构件的基板24时,通过控制基于离子发生器的吹送、湿度,能够进一步抑制有机硅树脂层14的残片静电吸附于带构件的基板24。
上述带构件的基板24的制造方法适于手机、PDA那样的移动终端中使用的小型显示装置的制造。显示装置主要为LCD或OLED,作为LCD,包含TN型、STN型、FE型、TFT型、MIM型、IPS型、VA型等。基本上无源驱动型、主动驱动型中的任意显示装置的情况下均可适用。
作为通过上述方法制造的带构件的基板24,可列举出具有玻璃基板和显示装置用构件的显示装置用面板、具有玻璃基板和太阳能电池用构件的太阳能电池、具有玻璃基板和薄膜二次电池用构件的薄膜二次电池、具有玻璃基板和接收传感器用构件的接收传感器面板、具有玻璃基板和电子器件用构件的电子部件等。作为显示装置用面板,包含液晶面板、有机EL面板、等离子体显示器面板、场发射面板等。作为接收传感器面板,包含电磁波接收传感器面板、X射线光接收传感器面板、紫外线光接收传感器面板、可见光光接收传感器面板、红外线光接收传感器面板等。
需要说明的是,上述对使用了玻璃层叠体10的电子器件的制造方法进行了详细叙述,但在使用了上述树脂层叠体的情况下,也可以通过同样的步骤实现电子器件的制造。
更具体而言,作为电子器件的制造方法的其它方式,可列举出具备如下工序的方案:使用带有机硅树脂层的树脂基板和支撑基材,形成树脂层叠体的工序;构件形成工序,在树脂层叠体的树脂基板的表面上形成电子器件用构件,得到带电子器件用构件的层叠体;及分离工序,从带电子器件用构件的层叠体将支撑基材及有机硅树脂层去除,得到具有树脂基板和电子器件用构件的电子器件。
形成树脂层叠体的工序可列举出包含上述树脂层形成工序2及层叠工序2的工序。
作为使用了树脂层叠体的情况下的构件形成工序及分离工序的步骤,可列举出与使用了玻璃层叠体的情况下的构件形成工序及分离工序同样的步骤。
需要说明的是,如上所述,由于树脂基板与有机硅树脂层的密合性比较弱,因此在分离工序中,相较于有机硅树脂层与支撑基材之间,树脂基板与有机硅树脂层之间更容易分离。特别是,使用玻璃板作为支撑基材的情况下,该倾向变得显著。
另外,上述说明中的使用了玻璃层叠体10的电子器件的制造方法中,使用半导体基板代替玻璃基板而形成的半导体层叠体也可以通过同样的步骤制造电子器件。
[实施例]
以下,通过实施例等具体地对本发明进行说明,但本发明不限制于这些例子。例1~18为实施例、例19及20为比较例。进而,例21为实施例、例22为比较例、例23~25为实施例、例26~28为比较例、例29为实施例、例30为比较例。
以下的实施例及比较例中,作为支撑基材,使用由无碱硼硅酸盐玻璃形成的玻璃板(长240mm、宽240mm、板厚0.5mm、线膨胀系数38×10-7/℃),作为玻璃基板,使用由无碱硼硅酸盐玻璃形成的玻璃板(长240mm、宽240mm、板厚0.2mm、线膨胀系数38×10-7/℃)。
[固化性有机硅1的合成]
在1L的烧瓶中加入三乙氧基甲基硅烷(179g)、甲苯(300g)、乙酸(5g),将混合物在25℃下搅拌20分钟后,进而,加热至60℃反应12小时。使得到的反应粗液冷却至25℃后,使用水(300g),将反应粗液清洗3次。
在经清洗的反应粗液中加入氯三甲基硅烷(70g),将混合物在25℃下搅拌20分钟后,进而,加热至50℃反应12小时。将得到的反应粗液冷却至25℃后,使用水(300g),将反应粗液清洗3次。
从经清洗的反应粗液中减压蒸馏去除甲苯,形成浆料状态后,在真空干燥机中进行整夜干燥,从而得到白色的有机聚硅氧烷化合物即固化性有机硅1。对于固化性有机硅1,T单元的个数:M单元的个数=87:13(摩尔比)。
<例1>
使固化性有机硅1溶解于异构烷烃系溶剂(IsoperG(TonenGeneral Sekiyu K.K制))后,对于得到的溶液以成为表1中记载的添加量的方式添加金属化合物及添加剂,使用搅拌转子(mix rotor)搅拌5分钟。需要说明的是,得到的组合物X中的固化性有机硅1的浓度为50质量%。
接着,通过旋转涂布法,以固化后的有机硅树脂层的厚度成为4μm的方式,在支撑基材上涂布组合物X,然后,在100℃下实施10分钟加热处理,形成涂膜。
接着,对形成有涂膜的支撑基材,在250℃下实施30分钟加热处理,形成有机硅树脂层。
然后,在室温下利用辊贴合机将玻璃基板和支撑基材的有机硅树脂层面贴合,得到玻璃层叠体。
得到的玻璃层叠体中,支撑基材和玻璃基板与有机硅树脂层不产生气泡地密合,也没有变形状缺陷。另外,在玻璃层叠体中,有机硅树脂层与支撑基材的层的界面的剥离强度大于玻璃基板的层与有机硅树脂层的界面的剥离强度。
<例2~17>
如表1~表3所示那样改变使用的金属化合物及添加剂的种类及用量,除此以外,按照与例1同样的步骤,得到玻璃层叠体。
需要说明的是,四正丙醇锆使用“Orgatics ZA-45”(Matsumoto Fine ChemicalCo.Ltd.制、金属含有率21.1%)。
另外,双(2-乙基己酸)锡(II)使用“Neostann U-28”(日东化成株式会社制、金属含有率29%)。
另外,新癸酸铋(III)使用“新癸酸铋16%”(日本化学产业株式会社制、金属含有率16%)。
<例18>
[固化性有机硅2的合成]
(有机氢硅氧烷的合成)
将1,1,3,3-四甲基二硅氧烷(5.4g)、四甲基环四硅氧烷(96.2g)、八甲基环四硅氧烷(118.6g)的混合物冷却至5℃,边搅拌混合液边将浓硫酸11.0g缓慢加入至混合液后,进而用1小时将水3.3g滴加至混合液中。边保持混合液的温度为10~20℃边搅拌8小时后,在混合液中加入甲苯,进行水洗及废酸分离直至硅氧烷层变为中性。对变为中性的硅氧烷层进行减压加热浓缩,去除甲苯等低沸点馏分,得到下述式(1)中k=40、l=40的有机氢硅氧烷。
(含烯基硅氧烷的合成)
在1,3-二乙烯基-1,1,3,3-四甲基二硅氧烷(3.7g)、1,3,5,7-四甲基-1,3,5,7-四乙烯基环四硅氧烷(41.4g)、八甲基环四硅氧烷(355.9g)中以Si/K=20000/1(mol比)量加入氢氧化钾的硅酸盐,在氮气气氛下在150℃下进行6小时平衡化反应。然后,添加相对于K(钾)为2mol量的2-氯乙醇,将混合液在120℃下进行2小时中和。然后,将得到的混合液在160℃、666Pa下进行6小时加热鼓泡处理,去掉挥发成分,得到平均100g的烯基当量数La=0.9、Mw:26000的含烯基硅氧烷。
将有机氢硅氧烷和含烯基硅氧烷以全部烯基与全部键合于硅原子的氢原子的摩尔比(氢原子/烯基)为0.9的方式进行混合,制备固化性有机硅2,在该固化性有机硅100质量份中混合下述式(2)所示的具有炔系不饱和基团的硅化合物1质量份,以成为表3中的含量的方式加入铂催化剂,得到混合物A。
HC≡C-C(CH3)2-O-Si(CH3)3 (2)
使混合物A溶解于八甲基四环硅氧烷(Dow Corning Toray Co.,Ltd.制、XIAMETERPMX-0244)后,对于得到的溶液以成为表3中记载的添加量的方式添加金属化合物,使用搅拌转子进行5分钟搅拌。需要说明的是,得到的组合物Y中的固化性有机硅2的浓度为30质量%。
接着,通过旋转涂布法,以固化后的有机硅树脂层的厚度成为8μm的方式在支撑基材上涂布组合物Y,然后,在140℃下实施10分钟加热处理,形成涂膜。
接着,对形成有涂膜的支撑基材在220℃下实施30分钟加热处理,形成有机硅树脂层。
然后,在室温下用辊贴合机将玻璃基板和支撑基材的有机硅树脂层面贴合,得到玻璃层叠体。
得到的玻璃层叠体中,支撑基材和玻璃基板与有机硅树脂层不产生气泡地密合,也没有变形状缺陷。另外,玻璃层叠体中,有机硅树脂层与支撑基材的层的界面的剥离强度大于玻璃基板的层与有机硅树脂层的界面的剥离强度。
<实施例18x~18z>
如表4所示那样改变使用的金属化合物的种类,按照与例18同样的步骤,得到玻璃层叠体。
<例19>
除了不使用金属化合物以外,按照与例1同样的步骤,得到玻璃层叠体。需要说明的是,例19的玻璃层叠体的有机硅树脂层中不含特定元素。
<例20>
不使用规定的金属化合物,将140℃的温度改变为100℃、将220℃的温度改变为250℃,除此以外,根据与例18同样的步骤,得到玻璃层叠体。需要说明的是,例20的玻璃层叠体的有机硅树脂层中不含特定元素。
[端部变质评价]
切取在各例中得到的玻璃层叠体,得到50×50mm的样品。将得到的各样品分别放入预热至450℃的电炉中,实施1小时加热处理后,取出样品。需要说明的是,电炉中的气氛为大气气氛。
使用显微镜,观察取出样品的端部,观察自端部起白化的部分的最大长度。需要说明的是,最大长度意指如图3所示那样的白化的端部的长度L中的最大值。表示端部变质的L的长度越短,效果越优异。
将结果汇总示于表1~表4。
[表1]
[表2]
[表3]
[表4]
如表1~表4所示,确认到本发明的层叠体表现出期望的效果。
其中,有机硅树脂层含有铁、锰、铜、铈、或铋作为特定元素的情况下,确认到更优异的效果。
另一方面,有机硅树脂层不含特定元素的例19及20中,效果差。
需要说明的是,确认到,在进行了上述端部变质评价后的例1~16的玻璃层叠体中的玻璃基板与有机硅树脂层的界面插入厚度0.1mm的不锈钢制刀具而形成剥离的切口部后,将玻璃基板完全固定,通过提起支撑基材能够容易地将玻璃基板剥离。
另一方面,关于添加四正丙醇锆且未添加双(2-乙基己酸)锡(II)的例17,剥离强度高,形成切口部后将玻璃基板完全固定并提起支撑基材时,有时产生支撑基材的破裂。
<例21及22>
使用例18及20的玻璃层叠体,将[端部变质评价]的温度由450℃改变为400℃,除此以外,按照同样的步骤,实施上述的端部变质评价。
需要说明的是,例22的玻璃层叠体的有机硅树脂层中不含特定元素。将结果示于表5。
需要说明的是,表5中,关于评价条件,示出端部变质评价中进行评价的温度及时间。
[表5]
如表5所示,确认到,在400℃下进行评价的情况下也是,本发明的层叠体(例21)与有机硅树脂层不含特定元素、不满足本发明的要件的层叠体(例22)相比,表现出有利的效果。
以下的例23~28中,对使用树脂基板即聚酰亚胺树脂基板作为基板来制作树脂层叠体的例子进行说明。
作为聚酰亚胺树脂基板,使用聚酰亚胺薄膜(厚度0.038mm、东洋纺株式会社制商品名“XENOMAX”)。
<例23>
使用聚酰亚胺树脂基板代替玻璃基板,除此以外,按照与例6同样的步骤,得到依次具备支撑基材、有机硅树脂层和聚酰亚胺树脂基板的树脂层叠体。
<例24>
使用聚酰亚胺树脂基板代替玻璃基板,除此以外,按照与例18同样的步骤,得到依次具备支撑基材、有机硅树脂层和聚酰亚胺树脂基板的树脂层叠体。
<例25>
将与例18同样地制备的组合物Y,以固化后的有机硅树脂层的厚度成为8μm的方式,用模涂法涂布于聚酰亚胺树脂基板,使用热板,在140℃下实施10分钟加热处理,形成涂膜。
接着,对形成有涂膜的聚酰亚胺树脂基板,在220℃下实施30分钟加热处理,形成有机硅树脂层。
接着,将支撑基材置于有机硅树脂层上,用辊贴合机进行贴合,得到树脂层叠体。
<例26>
不使用规定的金属化合物,除此以外,按照与例23同样的步骤,得到树脂层叠体。需要说明的是,例26的树脂层叠体的有机硅树脂层中不含特定元素。
<例27>
不使用规定的金属化合物,将140℃的温度改变为100℃、将220℃的温度改变为250℃,除此以外,按照与例24同样的步骤,得到树脂层叠体。需要说明的是,例27的树脂层叠体的有机硅树脂层中不含特定元素。
<例28>
不使用规定的金属化合物,将140℃的温度改变为100℃、将220℃的温度改变为250℃,除此以外,按照与例25同样的步骤,得到树脂层叠体。需要说明的是,例28的树脂层叠体的有机硅树脂层中不含特定元素。
[端部变质评价]
切取各例中得到的树脂层叠体,得到50×50mm的样品。将得到的各样品分别放入预热至400℃或450℃的电炉中,实施1小时加热处理后,取出样品。需要说明的是,电炉中的气氛为大气气氛。
使用显微镜,观察取出样品的端部,观察自端部起发生白化的部分的最大长度。需要说明的是,最大长度意指如图3所示那样的白化的端部的长度L中的最大值。表示端部变质的L的长度越短,效果越优异。
将结果汇总示于表6。
需要说明的是,表6中,“形成面”栏示出在支撑基材及聚酰亚胺树脂基板的哪个表面形成有机硅树脂层后制作树脂层叠体。
“评价条件”栏示出端部变质评价中进行评价的温度及时间。
另外,表6中,例24及例25的“评价条件”栏中所示的“400℃-1h及450℃-1h”表示“在400℃下1小时”及“在450℃下1小时”中的任一条件下“端部变质长度”均为“0.0mm”。
[表6]
如表6所示,确认到,本发明的层叠体即使在基板采用树脂基板的情况下,也表现出期望的效果。
另外,确认到,本发明的层叠体在树脂基板表面上形成有机硅树脂层来制造树脂层叠体的情况下,也表现出期望的效果。
另一方面,有机硅树脂层不含特定元素的例26~28中,效果差。
<例29>
代替例18中的长240mm、宽240mm、厚度0.2mm的玻璃基板,制作贴合直径150mm、厚度625μm的Si晶圆而成的层叠体。对该层叠体在与例18相同的条件下实施端部变质评价,结果端部变质长度为0.0mm。
<例30>
代替例20中的长240mm、宽240mm、厚度0.2mm的玻璃基板,制作贴合直径150mm、厚度625μm的Si晶圆而成的层叠体。对该层叠体在与例20相同的条件下实施端部变质评价,结果端部变质长度为3.0mm。
在例23~28的任意各例中得到的树脂层叠体中,支撑基材和聚酰亚胺树脂基板与有机硅树脂层不产生气泡地密合,也没有变形状缺陷。
另外,各例的树脂层叠体的任意者中均是:在端部变质评价的前后,有机硅树脂层与支撑基材的层的界面的剥离强度大于聚酰亚胺树脂基板的层与有机硅树脂层的界面的剥离强度。
需要说明的是,确认到:在例23~25的各树脂层叠体中的聚酰亚胺树脂基板与有机硅树脂层的界面插入厚度0.1mm的不锈钢制刀具而形成剥离的切口部后,将聚酰亚胺树脂基板完全固定,提起支撑基材,由此剥离聚酰亚胺树脂基板,结果有机硅树脂层未附着于被剥离的聚酰亚胺树脂基板。
另外,例29的层叠Si晶圆而成的层叠体中,有机硅树脂层与Si晶圆不产生气泡地密合,也没有变形状缺陷。另外确认到,在例29的Si晶圆与有机硅树脂层的界面插入厚度0.1mm的不锈钢制刀具而形成剥离的切口部后,将Si晶圆完全固定,提起支撑基材,由此来剥离Si晶圆,结果有机硅树脂层未附着于被剥离的Si晶圆。
本申请基于2016年12月28日提出的日本专利申请2016-255155、2017年6月20日提出的日本专利申请2017-120816及2017年9月27日提出的日本专利申请2017-186225,其内容作为参照并入此处。
Claims (15)
1.一种固化性组合物,其是用于贴合玻璃的固化性组合物,其中,
所述固化性组合物包含固化性有机硅和作为金属成分的锰元素,
所述金属成分的含量相对于所述固化性组合物形成的有机硅树脂层100质量份为0.001~1质量份。
2.根据权利要求1所述的固化性组合物,其中,所述金属成分的含量相对于所述固化性组合物形成的有机硅树脂层100质量份为0.01~0.7质量份。
3.根据权利要求1所述的固化性组合物,其中,所述金属成分以金属化合物的形式被包含。
4.根据权利要求3所述的固化性组合物,其中,所述金属化合物为络合物。
5.根据权利要求1所述的固化性组合物,其中,所述固化性有机硅的重均分子量为5000~60000。
6.根据权利要求1~5中的任一项所述的固化性组合物,其中,所述固化性组合物用于贴合包含半导体材料的基板与玻璃。
7.一种层叠体,其具备包含半导体材料的基板、和介由有机硅树脂层设置在所述基板上的玻璃,
所述有机硅树脂层包含有机硅树脂和作为金属成分的锰元素,
所述金属成分的含量相对于所述有机硅树脂层100质量份为0.001~1质量份。
8.根据权利要求7所述的层叠体,其中,所述金属成分的含量相对于所述有机硅树脂层100质量份为0.01~0.7质量份。
9.根据权利要求7所述的层叠体,其中,所述有机硅树脂层的厚度为0.001~50μm。
10.根据权利要求9所述的层叠体,其中,所述有机硅树脂层的厚度为0.001~10μm。
11.根据权利要求7~10中的任一项所述的层叠体,其中,所述基板包含LED。
12.一种带有机硅树脂层的玻璃,其具备有机硅树脂层和玻璃,
所述有机硅树脂层包含有机硅树脂和作为金属成分的锰元素、
所述金属成分的含量相对于所述有机硅树脂层100质量份为0.001~1质量份。
13.根据权利要求12所述的带有机硅树脂层的玻璃,其中,所述金属成分的含量相对于所述有机硅树脂层100质量份为0.01~0.7质量份。
14.根据权利要求12所述的带有机硅树脂层的玻璃,其中,所述有机硅树脂层的厚度为0.001~50μm。
15.根据权利要求14所述的带有机硅树脂层的玻璃,其中,所述有机硅树脂层的厚度为0.001~10μm。
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JP6934834B2 (ja) * | 2018-04-02 | 2021-09-15 | 富士フイルム株式会社 | 放射線画像撮影装置及びプログラム |
JP7103163B2 (ja) * | 2018-10-31 | 2022-07-20 | Agc株式会社 | 積層体、導通チェック方法、および、電子デバイスの製造方法 |
KR20220037436A (ko) * | 2019-07-25 | 2022-03-24 | 에이지씨 가부시키가이샤 | 적층 부재 |
WO2021015057A1 (ja) * | 2019-07-25 | 2021-01-28 | Agc株式会社 | 積層部材 |
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TW334469B (en) * | 1995-08-04 | 1998-06-21 | Doconitele Silicon Kk | Curable organosiloxane compositions and semiconductor devices |
JP4849814B2 (ja) * | 2005-03-29 | 2012-01-11 | 東レ・ダウコーニング株式会社 | ホットメルト型シリコーン系接着剤 |
CN101242951B (zh) | 2005-08-09 | 2012-10-31 | 旭硝子株式会社 | 薄板玻璃层压体以及利用薄板玻璃层压体的显示装置的制造方法 |
US20070077218A1 (en) * | 2005-08-26 | 2007-04-05 | L'oreal | Composition containing a coloring agent |
JP5562597B2 (ja) * | 2009-08-28 | 2014-07-30 | 荒川化学工業株式会社 | 支持体、ガラス基板積層体、支持体付き表示装置用パネル、および表示装置用パネルの製造方法 |
WO2012137976A1 (ja) * | 2011-04-08 | 2012-10-11 | 東レ・ダウコーニング株式会社 | 被膜形成用組成物 |
JP2013124324A (ja) * | 2011-12-15 | 2013-06-24 | Mitsubishi Chemicals Corp | 硬化性ポリオルガノシロキサン組成物および該組成物を硬化させてなるポリオルガノシロキサン硬化物 |
JP5978912B2 (ja) * | 2012-10-18 | 2016-08-24 | 旭硝子株式会社 | ガラス積層体の製造方法、電子デバイスの製造方法 |
WO2015060822A1 (en) * | 2013-10-22 | 2015-04-30 | Empire Technology Development Llc | Thermally printed optic circuits |
KR20160102429A (ko) * | 2013-12-27 | 2016-08-30 | 아사히 가라스 가부시키가이샤 | 유리 적층체 및 그 제조 방법 |
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CN108248159B (zh) | 2023-04-14 |
KR102475942B1 (ko) | 2022-12-08 |
US20180178492A1 (en) | 2018-06-28 |
KR102635001B1 (ko) | 2024-02-07 |
KR20230002139A (ko) | 2023-01-05 |
TWI751253B (zh) | 2022-01-01 |
TW201825288A (zh) | 2018-07-16 |
CN108248159A (zh) | 2018-07-06 |
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