CN109721752B - 玻璃布、预浸料以及印刷电路板 - Google Patents

玻璃布、预浸料以及印刷电路板 Download PDF

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CN109721752B
CN109721752B CN201811286553.2A CN201811286553A CN109721752B CN 109721752 B CN109721752 B CN 109721752B CN 201811286553 A CN201811286553 A CN 201811286553A CN 109721752 B CN109721752 B CN 109721752B
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glass cloth
mass
group
glass
silane coupling
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CN109721752A (zh
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柿崎宏昂
杉村昌治
立花信一郎
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Asahi Kasei Corp
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Asahi Kasei Corp
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    • C08J5/04Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/0405Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
    • C08J5/043Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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    • C03C13/00Fibre or filament compositions
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    • D06M15/55Epoxy resins
    • HELECTRICITY
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  • Chemical & Material Sciences (AREA)
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  • Microelectronics & Electronic Packaging (AREA)
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Abstract

本发明涉及玻璃布、预浸料以及印刷电路板。本发明的目的在于提供介电常数低、绝缘可靠性优异的玻璃布。一种玻璃布,其为对由多根玻璃单丝形成的玻璃丝进行织造而成的玻璃布,前述玻璃单丝中,B2O3组成量为15质量%~30质量%,SiO2组成量为45质量%~60质量%,P2O5组成量为2质量%~8质量%,前述玻璃布的灼烧失重值为0.90质量%~2.0质量%。

Description

玻璃布、预浸料以及印刷电路板
技术领域
本发明涉及玻璃布、预浸料以及印刷电路板。
背景技术
当今伴随着智能手机等情报终端的高性能化、高速通信化,在所使用的印刷电路板中,低介电常数化、低介电损耗角正切化显著推进。
作为该印刷电路板的绝缘材料,广泛使用层叠将玻璃布浸渗于环氧树脂等热固化性树脂(以下称为“基质树脂”)而得到的预浸料并使其加热加压固化而得到的层叠板。上述高速通信基板中所使用的基质树脂的介电常数为3左右,与之相对,通常的E玻璃布的介电常数为6.7左右,明显显现出来制成层叠板时的高介电常数的问题。
因此提出与E玻璃不同组成的D玻璃、NE玻璃、L玻璃等低介电常数玻璃布。通常对于低介电常数化需要增加玻璃组成中的SiO2与B2O3的配混量。
其中,增加B2O3的配混量时,玻璃熔融粘度降低,容易生产玻璃丝。此外,由于玻璃熔融粘度降低,拉拔玻璃丝时产生的玻璃丝内的气泡(以下称为“中空丝”)的量变少。该中空丝是对基板的绝缘可靠性劣化产生大幅影响的重要品质。
另一方面,增加B2O3的配混量时,产生玻璃的吸湿量会增加的问题。玻璃的吸湿量为对基板的绝缘可靠性劣化产生极大影响的因素,即便考虑降低上述中空丝的量也对基板的绝缘可靠性降低产生较大影响。对于该问题,公开了在玻璃布的表面附着0.25%以上的表面处理剂的方法等(例如,参照专利文献1)。
现有技术文献
专利文献
专利文献1:国际公开第2016/175248号
发明内容
发明要解决的问题
然而,伴随着下一代5G通信化等,在基板、树脂以及玻璃布中进一步要求低介电常数化。此外,需要改善树脂与玻璃布伴随低介电常数化的粘接性的降低以及绝缘可靠性的降低。
本发明鉴于上述问题而完成的,其目的在于提供介电常数低、绝缘可靠性优异的玻璃布。
用于解决问题的方案
本发明人等为了解决前述问题而进行了研究,结果发现构成玻璃布的玻璃单丝具有规定的B2O3组成量、SiO2组成量以及P2O5组成量并且玻璃布的灼烧失重值在规定的范围的玻璃布的介电常数低、绝缘可靠性优异,从而完成本发明。
即,本发明如以下所述。
[1]
一种玻璃布,其为对由多根玻璃单丝形成的玻璃丝进行织造而成的玻璃布,前述玻璃单丝中,B2O3组成量为15质量%~30质量%,SiO2组成量为45质量%~60质量%,P2O5组成量为2质量%~8质量%,前述玻璃布的灼烧失重值为0.90质量%~2.0质量%。
[2]
根据[1]所述的玻璃布,其利用下式(1)所示的硅烷偶联剂进行过表面处理。
X(R)3-nSiYn···(1)
(式(1)中,X为具有1个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,Y彼此独立地为烷氧基,n为1以上且3以下的整数,R彼此独立地为选自由甲基、乙基以及苯基组成的组中的基团。)
[3]
根据[1]所述的玻璃布,其利用由下式(2)所示的硅烷偶联剂进行过表面处理。
X(R)3-nSiYn···(2)
(式(2)中,X为具有3个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,Y彼此独立地为烷氧基,n为1以上且3以下的整数,R彼此独立地为选自由甲基、乙基以及苯基组成的组中的基团。)
[4]
根据[1]所述的玻璃布,其利用由下式(3)所示的硅烷偶联剂进行过表面处理。
X(R)3-nSiYn···(3)
(式(3)中,X为具有4个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,Y彼此独立地为烷氧基,n为1以上且3以下的整数,R彼此独立地为选自由甲基、乙基以及苯基组成的组中的基团。)
[5]
一种预浸料,其包含[1]~[4]中任一项所述的玻璃布和浸渗于该玻璃布的基质树脂。
[6]
一种印刷电路板,其使用[5]所述的预浸料而制作。
发明的效果
通过使用本发明的玻璃布,从而可以制作低介电常数且绝缘可靠性优异的预浸料以及印刷电路板。
具体实施方式
以下,对于本发明的实施方式(以下,称为“本实施方式”)进行详细地说明,但本发明不限于此,在不脱离其主旨的范围内可以进行各种变形。
〔玻璃布〕
本实施方式的玻璃布为对由多根玻璃单丝形成的玻璃丝进行织造而成的玻璃布。
前述玻璃单丝中,B2O3组成量为15质量%~30质量%,SiO2组成量为45质量%~60质量%,P2O5组成量为2质量%~8质量%。
此外,本实施方式的玻璃布的灼烧失重值为0.90质量%~2.0质量%。
通过使用本实施方式的玻璃布,从而与使用通常的E玻璃、D玻璃、NE玻璃以及L玻璃组成的玻璃布而得到的层叠板相比介电常数进一步降低。
玻璃单丝中,B2O3组成量为15质量%~30质量%,优选为20质量%~27质量%,更优选为21质量%~25质量%。
B2O3组成量为15质量%以上,从而玻璃熔融粘度降低,容易拉拔玻璃丝,因此可以使玻璃布的中空丝品质稳定化。此外,B2O3组成量为30质量%以下,从而在实施过表面处理的情况下,耐吸湿性进一步提高。
玻璃单丝中,SiO2组成量为45质量%~60质量%,优选为47质量%~58质量%,更优选为50质量%~55质量%。
SiO2组成量为45%以上,从而所得到的层叠板的介电常数变低。此外,SiO2组成量为60%以下,从而所得到的层叠板的钻孔加工性进一步提高。
玻璃单丝中,P2O5组成量为2质量%~8质量%,优选为3质量%~7质量%,更优选为3质量%~6质量%。
P2O5组成量为2质量%以上,从而可以进一步使玻璃布低介电常数化。此外,P2O5组成量为8质量%以下,从而在实施过表面处理的情况下,耐热性进一步提高。
本实施方式的玻璃布以及构成该玻璃布的玻璃单丝中的各成分的组成可以通过各成分的原料投入比来调整。此外,各成分的组成量通过公知的分析方法,例如可以通过荧光X射线分析/等离子体发光分析等组合评价而求出。
此外,玻璃单丝除B2O3、SiO2、P2O5以外还可以具有其它成分。作为其它成分没有特别限定,例如可以列举出Al2O3、CaO、MgO等。
玻璃单丝中,Al2O3组成量优选为10质量%~20质量%,更优选为13质量%~19质量%。Al2O3组成量为上述范围内,从而存在丝的生产率进一步提高的倾向。
玻璃单丝中,CaO组成量优选为0质量%~8质量%,更优选为1质量%~8质量%。CaO组成量为上述范围内,从而存在丝的生产率进一步提高的倾向。
玻璃单丝中,MgO组成量优选为0质量%~5质量%,更优选为1质量%~5质量%。MgO组成量为上述范围内,从而存在丝的生产率进一步提高的倾向。
本实施方式中的玻璃单丝的组成优选的是B2O3、SiO2、P2O5、以及上述的其它成分总计为100质量%。
玻璃单丝的平均长丝直径优选为2.5μm~9.0μm,更优选为3.5μm~7.0μm。玻璃单丝的平均长丝直径为上述范围内,从而将所得到的层叠板利用机械钻、二氧化碳激光、UV-YAG激光进行加工时,存在加工性进一步提高的倾向。
构成玻璃布的经丝以及纬丝的排列密度优选为10根/英寸~120根/英寸,更优选为40根/英寸~100根/英寸。
此外,玻璃布的布重量(单位面积重量)优选为8g/m2~250g/m2,更优选为8g/m2~100g/m2
进而,用表面处理剂处理之前的玻璃布的厚度优选为7μm~100μm。
对于玻璃布的编织结构没有特别限定,例如,可以列举出平纹组织、方平组织、缎纹组织、斜纹组织等编织结构。其中,优选平纹组织结构。
本实施方式的玻璃布以及构成该玻璃布的玻璃单丝为用表面处理剂进行了处理的丝。
作为表面处理剂没有特别限定,例如,可以适宜地列举出硅烷偶联剂。玻璃布的基于表面处理剂的处理量可以用以下的灼烧失重值来估算。
玻璃布的灼烧失重值为0.90质量%~2.0质量%,优选为0.95质量%~1.8质量%,更优选为0.95质量%~1.5质量%。
玻璃布的灼烧失重值为0.90质量%以上,从而制造层叠板时,可以得到足够的与基质树脂的粘接性,此外,耐吸湿性进一步提高。此外,玻璃布的灼烧失重值为2.0质量%以下,从而树脂向玻璃布的浸透性进一步提高。
在此,所谓“灼烧失重值”是指基于JISR3420中记载的方法而测定的。即,首先将玻璃布投入到105℃±5℃的干燥机之中,至少干燥30分钟。干燥后,将玻璃布移至干燥器,自然冷却至室温。自然冷却后,以0.1mg以下的单位测量玻璃布。接着,在马弗炉中以625±20℃或在500~600℃中选择的温度加热玻璃布。625±20℃的情况下加热10分钟以上,在500~600℃中选择的温度的情况下,加热1小时以上。在马弗炉中加热后,将玻璃布移至干燥器,自然冷却至室温。自然冷却后,以0.1mg以下的单位测量玻璃布。用通过以上的测定方法求出的灼烧失重值来定义玻璃布的基于表面处理剂的处理量。
在本实施方式中,具体而言,可以根据以下的方法算出灼烧失重值。
首先,将玻璃布投入到110℃的干燥机之中,进行60分钟干燥。干燥后,将玻璃布移至干燥器,放置20分钟,自然冷却至室温。自然冷却后,以0.1mg以下的单位测量玻璃布。接着,在马弗炉中以625℃对玻璃布进行20分钟加热。在马弗炉中加热后,将玻璃布移至干燥器,放置20分钟,自然冷却至室温。自然冷却后,以0.1mg以下的单位测量玻璃布。用通过以上的测定方法求出的灼烧失重值来定义玻璃布的硅烷偶联剂处理量。
作为将本实施方式中的灼烧失重值设为0.90质量%~2.0质量%的方法,例如,可以列举出利用表面处理剂处理进行表面处理之前的玻璃布时,调整表面处理液中的表面处理剂的浓度的方法;利用将玻璃布浸渍于表面处理液的时间和/或基于压液辊等的挤压压力来进行调整的方法;将表面处理剂向玻璃布加热固着的方法;利用高压喷射水等对利用处理剂进行处理之后的玻璃布进行清洗的方法等。这些方法可以仅使用1种也可以组合使用2种以上。
作为表面处理剂之一的硅烷偶联剂没有特别限定,例如,优选使用由下述式(1)所示的硅烷偶联剂。通过使用由式(1)所示的硅烷偶联剂,存在耐吸湿性进一步提高的倾向。需要说明的是,在玻璃布的制造方法中,将硅烷偶联剂涂布到玻璃布时,优选用使硅烷偶联剂溶解或分散于溶剂中而成的处理液(以下,简称为“处理液”)来进行处理的方法。
X(R)3-nSiYn···(1)
式(1)中,X为具有1个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,Y彼此独立地为烷氧基,n为1以上且3以下的整数,R彼此独立地为选自由甲基、乙基以及苯基组成的组中的基团。
X更优选为具有3个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,进一步优选具有4个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团。X为这样的官能团,从而具有耐吸湿性进一步提高的倾向。
将式(1)中的X为具有3个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团的情况下的硅烷偶联剂称为式(2)所示的硅烷偶联剂。
将式(1)中的X为具有4个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团的情况下的硅烷偶联剂称为式(3)所示的硅烷偶联剂。
本实施方式中的式(1)~(3)中的氨基可以为伯氨基(-NH2)、仲氨基(-NH-),叔氨基(-N<),包括这些伯氨基、仲氨基、叔氨基的任意者。
作为上述的烷氧基,可以使用任何形态,但为了向玻璃布的稳定处理化,优选碳数5以下的烷氧基。
作为具体地可以使用的硅烷偶联剂没有特别限定,例如,可以列举出N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷以及其的盐酸盐、N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基甲基二甲氧基硅烷以及其的盐酸盐、N-β-(N-二(乙烯基苄基)氨基乙基)-γ-氨基丙基三甲氧基硅烷以及其的盐酸盐、N-β-(N-二(乙烯基苄基)氨基乙基)-N-γ-(N-乙烯基苄基)-γ-氨基丙基三甲氧基硅烷以及其的盐酸盐、氨基丙基三甲氧基硅烷、(氨基乙基氨基)丙基三甲氧基硅烷、乙烯基三甲氧基硅烷、甲基丙烯酰氧基丙基三甲氧基硅烷、丙烯酰氧基丙基三甲氧基硅烷等公知的单体或它们的混合物。
作为使硅烷偶联剂溶解或分散的溶剂,可以使用水或有机溶剂的任意者,但从安全性、地球环境保护的观点出发,优选以水为主溶剂。作为得到以水为主溶剂的处理液的方法,优选将硅烷偶联剂直接投入到水中的方法、使硅烷偶联剂溶解于水溶性有机溶剂而制成有机溶剂溶液之后将该有机溶剂溶液投入到水中的方法的任意方法。
此外,为了提高硅烷偶联剂的处理液中的水分散性、稳定性,也可以并用表面活性剂。
〔玻璃布的制造方法〕
本实施方式的玻璃布的制造方法没有特别限定,例如,可以列举出具有如下工序的方法:利用浓度0.10质量%~3.0质量%的处理液,使硅烷偶联剂大致完全地覆盖玻璃单丝的表面的被覆工序;通过加热干燥使硅烷偶联剂固着于玻璃单丝的表面的固着工序;和利用高压喷射水等清洗在玻璃单丝的表面固着的硅烷偶联剂的至少一部分,从而以使灼烧失重值为0.90质量%~2.0质量%的范围的方式调整硅烷偶联剂的附着量的调制工序。
认为通过上述制造方法,可以在构成玻璃丝的每一根玻璃单丝的整个表面上大致完全并且均匀地形成硅烷偶联剂层。
作为将处理液涂布到玻璃布的方法,可以为(1)使处理液储存在浴槽中,使玻璃布浸渍、通过的方法(以下,称为“浸渍法”);(2)用辊涂机、模涂机或凹版涂布机等将处理液直接涂布到玻璃布的方法等。用上述(1)的浸渍法进行涂布的情况下,优选将玻璃布在处理液中的浸渍时间选定为0.5秒以上且1分钟以下。
此外,作为将处理液涂布到玻璃布之后,使溶剂加热干燥的方法,可以列举出暖风、电磁波等公知的方法。
加热干燥温度为了使硅烷偶联剂与玻璃的反应充分地进行,优选90℃以上、更优选100℃以上。此外,为了防止硅烷偶联剂具有的有机官能团的劣化,优选300℃以下,更优选200℃以下。
〔预浸料〕
本实施方式的预浸料包含上述玻璃布和浸渗于该玻璃布的基质树脂。由此,可以提供实现介电常数低、由中空丝减少带来的绝缘可靠性提高和由耐吸湿性提高带来的绝缘可靠性提高的预浸料。
作为基质树脂,可以使用热固化性树脂、热塑性树脂的任意者。
作为热固化性树脂,可以例示出:a)无催化剂或添加咪唑化合物、叔胺化合物、脲化合物、磷化合物等具有反应催化能力的催化剂而使具有环氧基的化合物和具有与环氧基反应的氨基、酚基、酸酐基、酰肼基、异氰酸酯基、氰酸酯基、羟基等的化合物反应来进行固化的环氧树脂;b)将热分解型催化剂或光分解型催化剂用作反应引发剂而使具有烯丙基、甲基丙烯基、丙烯基的化合物进行固化的自由基聚合型固化树脂;c)使具有氰酸酯基的化合物与具有马来酰亚胺基的化合物反应来进行固化的马来酰亚胺三嗪树脂;d)马来酰亚胺化合物与胺化合物反应来进行固化的热固化性聚酰亚胺树脂;e)通过加热聚合使具有苯并噁嗪环的化合物进行交联固化的苯并噁嗪树脂等。
此外,作为热塑性树脂,可以例示出聚苯醚、改性聚苯醚、聚苯硫醚、聚砜、聚醚砜、聚芳酯、芳香族聚酰胺、聚醚醚酮、热塑性聚酰亚胺、不溶性聚酰亚胺、聚酰胺酰亚胺、氟树脂等。此外,可以并用热固化性树脂和热塑性树脂。
〔印刷电路板〕
本实施方式的印刷电路板为使用上述预浸料而制作的。由此,可以提供介电常数低、绝缘可靠性优异的印刷电路板。
实施例
接着,通过实施例、比较例更详细地说明本发明。本发明并不限于以下的实施例。
需要说明的是,在任意的实施例以及比较例中,灼烧失重值通过如下操作来调整:将处理液中的表面处理剂的浓度适宜地调整为0.10质量%~3.0质量%的范围,適宜调整将玻璃布浸渍于表面处理液的时间和/或基于压液辊等的挤压压力,通过加热干燥使硅烷偶联剂固着于玻璃单丝的表面的固着工序,和利用高压水开纤清洗在玻璃单丝的表面固着的硅烷偶联剂。
(实施例1)
将B2O3为16质量%、SiO2为59质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.95质量%。
(实施例2)
将B2O3为25质量%、SiO2为52质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.96质量%。
(实施例3)
将B2O3为29质量%、SiO2为50质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.99质量%。
(实施例4)
将B2O3为25质量%、SiO2为52质量%、P2O5为7质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为1.3质量%。
(实施例5)
将B2O3为25质量%、SiO2为52质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为1.3质量%。
(实施例6)
将B2O3为25质量%、SiO2为52质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸,厚度46μm)浸渍于使(氨基丙基)三乙氧基硅烷(Dow Corning Toray Co.,Ltd.制;Z6011)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.91质量%。
(实施例7)
将B2O3为25质量%、SiO2为52质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使(氨基乙基氨基)丙基三甲氧基硅烷(Dow Corning Toray Co.,Ltd.制;Z6020)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.92质量%。
(比较例1)
将B2O3为14质量%、SiO2为61质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.90质量%。
(比较例2)
将B2O3为31质量%、SiO2为44质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.93质量%。
(比较例3)
将B2O3为25质量%、SiO2为52质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.80质量%。
(比较例4)
将B2O3为25质量%、SiO2为52质量%、P2O5为4质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为2.1质量%。
(比较例5)
将B2O3为25质量%、SiO2为52质量%、P2O5为9质量%的玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为1.3质量%。
(比较例6)
将B2O3为7质量%、SiO2为54质量%的E玻璃布(牌号1078:平均长丝直径5μm、经丝的排列密度54根/英寸、纬丝的排列密度54根/英寸、厚度46μm)浸渍于使N-β-(N-乙烯基苄基氨基乙基)-γ-氨基丙基三甲氧基硅烷的盐酸盐(Dow Corning Toray Co.,Ltd.制;Z6032)分散于水中而成的处理液中,进行加热干燥。接着,用喷雾器实施高压水开纤,进行加热干燥,得到玻璃布。硅烷偶联剂的灼烧失重值为0.24质量%。
<灼烧失重值的评价方法>
根据JISR3420中记载的方法,测定灼烧失重值。具体而言,将玻璃布投入到110℃的干燥机之中,进行60分钟干燥。干燥后,将玻璃布移至干燥器中,放置20分钟,自然冷却至室温。自然冷却后,以0.1mg以下的单位测量玻璃布。接着,用马弗炉以625℃将玻璃布加热20分钟。在马弗炉中加热后,将玻璃布移至干燥器中,放置20分钟,自然冷却至室温。自然冷却后,以0.1mg以下的单位测量玻璃布。测定马弗炉的加热前后的重量变化,作为处理剂附着量计算灼烧失重值。
<层叠板的作制方法>
在上述的实施例以及比较例中得到的玻璃布中浸渗环氧树脂清漆(低溴化双酚A型环氧树脂40质量份、邻甲酚型酚醛清漆环氧树脂10质量份、二甲基甲酰胺50质量份、双氰胺1质量份以及2-乙基-4-甲基咪唑0.1质量份的混合物),在160℃下进行2分钟干燥后得到预浸料。重叠该预浸料,进而,在上下方向上重叠厚度12μm的铜箔,以175℃、40kg/cm2进行60分钟加热加压,得到层叠板。
<层叠板的介电常数的评价方法>
如上述操作,以厚度1mm的方式制作层叠板,去除铜箔,得到用于介电常数评价的试样。使用阻抗分析仪(Agilent Technologies公司制)测定所得到的试样的频率1GHz下的介电常数。
<层叠板的吸水率、耐热性的评价方法>
如上述操作,以厚度0.4mm的方式制作层叠板,去除铜箔,得到用于吸水性评价的试样。将所得到的试样在120℃下加热60分钟,在干燥器中自然冷却至室温,用电子天平测定重量。接着,在压力锅容器中使其进行121℃500小时加热吸水,在水中自然冷却至室温之后,去除表面的水分,用电子天平测定重量。根据加热吸水前后的重量变化求出层叠板的吸水率。进而,将吸水后的层叠板在288℃的焊料浴中浸渍20秒,目视确认有无层叠板的裂纹。表1中,对于耐热性,没有裂纹时用○表示,具有裂纹时用×表示。没有裂纹是指耐热性优异。
<层叠板的粘接性的评价方法>
如上述那样操作,以成为厚度0.4mm的方式制作层叠板,用试验机AUTOGRAPH剥离层间中央部,求出粘接强度(kN/m)。
<层叠板的绝缘可靠性的评价方法>
如上述那样操作,以成为厚度0.4mm的方式制作层叠板,制作在层叠板的两面的铜箔上配置有0.15mm间隔的通孔的布线图案,得到绝缘可靠性评价的试样。对于所得到的试样,在温度120℃湿度85%RH的气氛下施加10V的电压,测定电阻值的变化。此时,将在试验开始后500小时以内电阻不足1MΩ的情况作为绝缘不良来计数。对于10枚试样,进行同样的测定,算出10枚中未成为绝缘不良的样品的比例。
在表1中总结示出实施例1~7与比较例1~6中示出的层叠板的介电常数、吸水率、耐热性、粘接性、绝缘可靠性评价结果。
表1
Figure BDA0001849177090000151
可知实施例1~7的玻璃布为低介电常数且吸水率、耐热性、粘接性、绝缘可靠性非常优异。
产业上的可利用性
本发明的玻璃布作为在电子以及电气领域中所使用的印刷电路板中所使用的基材具有产业上的可利用性。

Claims (6)

1.一种玻璃布,其为对由多根玻璃单丝形成的玻璃丝进行织造而成的玻璃布,所述玻璃单丝中,B2O3组成量为15质量%~30质量%,SiO2组成量为45质量%~60质量%,P2O5组成量为2质量%~8质量%,所述玻璃布的灼烧失重值为1.3质量%~2.0质量%。
2.根据权利要求1所述的玻璃布,其利用由下式(1)所示的硅烷偶联剂进行过表面处理,
X(R)3-nSiYn···(1)
式(1)中,X为具有1个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,Y彼此独立地为烷氧基,n为1以上且3以下的整数,R彼此独立地为选自由甲基、乙基以及苯基组成的组中的基团。
3.根据权利要求1所述的玻璃布,其利用由下式(2)所示的硅烷偶联剂进行过表面处理,
X(R)3-nSiYn···(2)
式(2)中,X为具有3个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,Y彼此独立地为烷氧基,n为1以上且3以下的整数,R彼此独立地为选自由甲基、乙基以及苯基组成的组中的基团。
4.根据权利要求1所述的玻璃布,其利用由下式(3)所示的硅烷偶联剂进行过表面处理,
X(R)3-nSiYn···(3)
式(3)中,X为具有4个以上的由氨基以及不饱和双键基团中选择的至少一者的有机官能团,Y彼此独立地为烷氧基,n为1以上且3以下的整数,R彼此独立地为选自由甲基、乙基以及苯基组成的组中的基团。
5.一种预浸料,其包含权利要求1~4中任一项所述的玻璃布和浸渗于该玻璃布的基质树脂。
6.一种印刷电路板,其使用权利要求5所述的预浸料而制作。
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