CN113039226A - 树脂组合物、光纤以及光纤的制造方法 - Google Patents
树脂组合物、光纤以及光纤的制造方法 Download PDFInfo
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- CN113039226A CN113039226A CN201980069824.5A CN201980069824A CN113039226A CN 113039226 A CN113039226 A CN 113039226A CN 201980069824 A CN201980069824 A CN 201980069824A CN 113039226 A CN113039226 A CN 113039226A
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- resin composition
- meth
- acrylate
- resin layer
- optical fiber
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- 239000013307 optical fiber Substances 0.000 title claims description 44
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- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 98
- 239000002245 particle Substances 0.000 claims abstract description 55
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 50
- 239000000178 monomer Substances 0.000 claims abstract description 24
- 238000012986 modification Methods 0.000 claims abstract description 14
- 230000004048 modification Effects 0.000 claims abstract description 14
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 24
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- 230000001678 irradiating effect Effects 0.000 claims description 4
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Abstract
一种树脂组合物,包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂的基础树脂;以及具有碳原子数为1以上8以下的烷基或苯基的表面修饰无机氧化物粒子,以树脂组合物的总量为基准,表面修饰无机氧化物粒子的含量为1质量%以上60质量%以下,表面修饰无机氧化物粒子中的表面修饰量为0.15mg/m2以上。
Description
技术领域
本发明涉及树脂组合物、光纤以及光纤的制造方法。
本专利申请要求基于2018年11月16日提出的日本专利申请第2018-215714号的优先权,并且援引了所述日本专利申请所记载的全部记载内容。
背景技术
通常,光纤具有用于保护作为光传输体的玻璃纤维的被覆树脂层。为了减小对光纤施加侧压时发生的微小弯曲所引起的传输损耗的增加,要求光纤具有优异的侧压特性。
例如,在专利文献1中,研究了通过使用含有以合成石英为原料的填料的紫外线固化型树脂组合物来形成树脂层,从而改善光纤的侧压特性。
现有技术文献
专利文献
专利文献1:日本特开2014-219550号公报
发明内容
本发明的一个方式涉及的树脂组合物包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂的基础树脂;以及具有碳原子数为1以上8以下的烷基或苯基的表面修饰无机氧化物粒子,以树脂组合物的总量为基准,表面修饰无机氧化物粒子的含量为1质量%以上60质量%以下,表面修饰无机氧化物粒子中的表面修饰量为0.15mg/m2以上。
附图说明
[图1]图1是表示本实施方式涉及的光纤的一个例子的示意性剖面图。
具体实施方式
[本发明要解决的课题]
被覆树脂层一般具备初级树脂层和次级树脂层。在形成次级树脂层的树脂组合物中,需要通过提高杨氏模量来提高光纤的侧压特性。然而,当填料的含量增加时,虽然可以提高由树脂组合物形成的树脂层的杨氏模量,但涂布性倾向于不足、树脂层倾向于变脆。
本发明的目的在于提供具有次级树脂层所需要的高杨氏模量、并且涂布性优异、可以形成强韧的树脂层的树脂组合物,以及具备由该树脂组合物形成的次级树脂层的光纤。
[本发明的效果]
根据本发明,能够提供具有次级树脂层所需要的高杨氏模量,并且涂布性优异、可以形成强韧的树脂层的光纤被覆用的树脂组合物,以及具备由该树脂组合物形成的次级树脂层的光纤。
[本发明实施方式的说明]
首先,列举本发明的实施方式的内容并进行说明。本发明的一个方式涉及的树脂组合物包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂的基础树脂;以及具有碳原子数为1以上8以下的烷基或苯基的表面修饰无机氧化物粒子,以树脂组合物的总量为基准,表面修饰无机氧化物粒子的含量为1质量%以上60质量%以下,表面修饰无机氧化物粒子中的表面修饰量为0.15mg/m2以上。
通过以特定的范围使用上述表面修饰无机氧化物粒子,可以形成具有高杨氏模量,并且涂布性优异的强韧的树脂层。
从在树脂组合物中的分散性优异、容易提高涂布性的观点来看,表面修饰无机氧化物粒子中的表面修饰量可以为0.15mg/m2以上2.5mg/m2以下。
碳原子数为1以上8以下的烷基可以是选自由甲基、乙基、丙基、丁基、戊基、己基以及辛基构成的组中的至少1种基团。由此,容易形成杨氏模量高的树脂层。
从形成杨氏模量高的树脂层的观点来看,表面修饰无机氧化物粒子的平均一次粒径可以为800nm以下。
本发明的一个方式涉及的光纤的次级被覆材料包含所述树脂组合物。通过将本实施方式涉及的树脂组合物用于次级树脂层,可以制作出侧压特性优异的光纤。
本发明的一个方式涉及的光纤具备:含有芯部和包层的玻璃纤维、与玻璃纤维接触并被覆该玻璃纤维的初级树脂层、以及被覆初级树脂层的次级树脂层,其中次级树脂层由所述树脂组合物的固化产物构成。通过将本实施方式涉及的树脂组合物应用于次级树脂层,能够提高光纤的侧压特性。
本发明的一个方式涉及的光纤的制造方法包括:将所述树脂组合物涂布在由芯部和包层构成的玻璃纤维的外周的涂布工序;以及在涂布工序之后通过照射紫外线使树脂组合物固化的固化工序。由此,可以制作出侧压特性优异的光纤。
[本发明实施方式的详细说明]
根据需要参照附图对本发明实施方式涉及的树脂组合物以及光纤的具体例子进行说明。需要说明的是,本发明不限于这些示例,而是由权利要求书所表示,并且意图包括与权利要求书等同的意义和范围内的所有变化。在下述说明中,在附图的说明中相同的要素标注相同的符号,并且省略重复的说明。
<树脂组合物>
本实施方式涉及的树脂组合物包括:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂的基础树脂;以及具有碳原子数为1以上8以下的烷基或苯基的表面修饰无机氧化物粒子。
这里,所谓(甲基)丙烯酸酯,指的是丙烯酸酯或与其相对应的甲基丙烯酸酯。这也同样地适用于(甲基)丙烯酸。
(表面修饰无机氧化物粒子)
本实施方式涉及的表面修饰无机氧化物粒子是通过具有碳原子数为1以上8以下的烷基或苯基的硅烷化合物对无机氧化物粒子的表面进行处理,从而在无机氧化物粒子的表面导入碳原子数为1以上8以下的烷基或苯基。即,表面修饰无机氧化物粒子由无机成分和有机成分构成。
具有碳原子数为1以上8以下的烷基或苯基的表面修饰无机氧化物粒子可以提高与基础树脂的相溶性,从而容易形成杨氏模量高的树脂层。另一方面,具有碳原子数为9以上的烷基的表面修饰无机氧化物粒子的亲油性较大,因此难以分散在树脂组合物中。碳原子数为1以上8以下的烷基可以是选自由甲基、乙基、丙基、丁基、戊基、己基以及辛基构成的组中的至少1种基团。
作为具有碳原子数为1以上8以下的烷基的硅烷化合物,例如可以列举出:甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙基三甲氧基硅烷、丙基三甲氧基硅烷、丁基三甲氧基硅烷、戊基三甲氧基硅烷、己基三甲氧基硅烷、辛基三甲氧基硅烷、甲基三乙氧基硅烷、二甲基二乙氧基硅烷、乙基三乙氧基硅烷、丙基三乙氧基硅烷、丁基三乙氧基硅烷、戊基三乙氧基硅烷、己基三乙氧基硅烷以及辛基三乙氧基硅烷。
作为具有苯基的硅烷化合物,例如可以列举出苯基三甲氧基硅烷和苯基三乙氧基硅烷。
本实施方式涉及的表面修饰无机氧化物粒子分散在分散介质中。通过使用分散在分散介质中的表面修饰无机氧化物,可以使表面修饰无机氧化物粒子均匀地分散在树脂组合物中,从而能够提高树脂组合物的保存稳定性。作为分散介质,只要其不妨碍树脂组合物的固化,则没有特别地限定。分散介质可以为反应性的,也可以为非反应性的。利用X射线小角散射法测定含有表面修饰无机氧化物粒子的分散介质,在没有测定到聚集的粒子的情况下,可以认为表面修饰无机氧化物粒子以一次粒子的形式分散。
作为反应性的分散介质,可以使用(甲基)丙烯酰基化合物、环氧化合物等单体。作为(甲基)丙烯酰基化合物,例如可以列举出:1,6-己二醇二(甲基)丙烯酸酯、EO改性双酚A二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、PO改性双酚A二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、聚四亚甲基二醇二(甲基)丙烯酸酯、2-羟基-3-苯氧基丙基(甲基)丙烯酸酯、丙二醇二缩水甘油醚的(甲基)丙烯酸加成物、三丙二醇二缩水甘油醚的(甲基)丙烯酸加成物、以及丙三醇二缩水甘油醚的(甲基)丙烯酸加成物。作为分散介质,也可以使用后述单体中示例的(甲基)丙烯酰基化合物。
作为非反应性的分散介质,可以使用甲基乙基酮(MEK)等酮类溶剂;甲醇(MeOH)、丙二醇单甲醚(PGME)等醇类溶剂;或者丙二醇单甲醚醋酸酯(PGMEA)等酯类溶剂。在使用非反应性的分散介质的情况下,在将基础树脂和分散在分散介质中的表面修饰无机氧化物粒子混合后,可以除去分散介质的一部分,从而制备树脂组合物。
从在树脂组合物中的分散性优异、并且容易形成平滑的树脂层的方面来看,上述表面修饰无机氧化物粒子优选为使选自由二氧化硅(氧化硅)、二氧化锆(氧化锆)、氧化铝(alumina)、氧化镁(magnesia)、氧化钛(titania)、氧化锡以及氧化锌构成的组中的至少1种经过表面处理后的粒子。从价格低廉、容易进行表面处理、具有紫外线透过性、容易对树脂层赋予适度的硬度等观点来看,更优选使用表面修饰氧化硅粒子作为本实施方式涉及的表面修饰无机氧化物粒子。
从提高树脂层的杨氏模量的观点来看,表面修饰无机氧化物粒子的平均一次粒径可以为800nm以下、优选为1nm以上650nm以下、更优选为5nm以上500nm以下、进一步优选为10nm以上200nm以下、特别优选为10nm以上100nm以下。平均一次粒径例如可以利用电子显微镜照片的图像分析、光散射法、BET法等来进行测定。在一次粒子的粒径较小的情况下,分散有表面修饰无机氧化物粒子的一次粒子的分散介质在目视下看起来是透明的。在一次粒子的粒径比较大(40nm以上)的情况下,分散有一次粒子的分散介质看起来是白浊的,但没有观察到沉淀物。
以树脂组合物的总量(基础树脂和表面修饰无机氧化物粒子的总量)为基准,表面修饰无机氧化物粒子的含量为1质量%以上60质量%以下、优选为3质量%以上55质量%以下、更优选为5质量%以上50质量%以下、进一步优选为10质量%以上40质量%以下。当表面修饰无机氧化物粒子的含量为1质量%以上时,容易形成侧压特性优异的树脂层。当表面修饰无机氧化物粒子的含量为60质量%以下时,容易提高树脂组合物的涂布性,且可以形成强韧的树脂层。需要说明的是,也可以认为树脂组合物的总量与树脂组合物的固化产物的总量相同。以次级树脂层的总量(构成次级树脂层的树脂组合物的固化产物的总量)为基准,表面修饰无机氧化物粒子的含量为1质量%以上60质量%以下、优选为3质量%以上55质量%以下、更优选为5质量%以上50质量%以下、进一步优选为10质量%以上40质量%以下。
表面修饰无机氧化物粒子中的表面修饰量为0.15mg/m2以上、优选为0.15mg/m2以上2.5mg/m2以下、更优选为0.20mg/m2以上2.0mg/m2以下、进一步优选为0.25mg/m2以上1.8mg/m2以下、特别优选为0.30mg/m2以上1.5mg/m2以下。通过使表面修饰量在上述范围内,容易调节树脂组合物的粘度。
本说明书中的“表面修饰量”可以根据表面修饰无机氧化物粒子的比表面积和有机成分的比例来算出。上述有机成分是源自导入到表面修饰前的无机氧化物粒子中的紫外线固化性官能团的成分。例如,在表面修饰无机氧化物粒子由氧化硅粒子构成的情况下,除SiO2以外的成分成为有机成分。可以利用氮吸附BET法测定比表面积,并且利用差热/热重分析法(TG/DTA)来测定有机成分的比例。表面修饰无机氧化物粒子中的表面修饰量可以在制备树脂组合物之前将粒子从分散介质中分离出来进行测定,也可以在制备树脂组合物之后将粒子从树脂组合物中分离出来进行测定。
(基础树脂)
本实施方式涉及的基础树脂含有:氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂。
作为氨基甲酸酯(甲基)丙烯酸酯低聚物,可以使用由多元醇化合物、多异氰酸酯化合物以及含羟基的(甲基)丙烯酸酯化合物进行反应而得到的低聚物。
作为多元醇化合物,例如可以列举出:聚四亚甲基二醇、聚丙二醇以及双酚A-环氧乙烷加成二醇。作为多异氰酸酯化合物,例如可以列举出:2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、异佛尔酮二异氰酸酯以及二环己基甲烷4,4’-二异氰酸酯。作为含羟基的(甲基)丙烯酸酯化合物,例如可以列举出:(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丁酯、1,6-己二醇单(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、(甲基)丙烯酸2-羟丙酯以及三丙二醇单(甲基)丙烯酸酯。
从调节树脂层的杨氏模量的观点来看,多元醇化合物的数均分子量可以为300以上3000以下。
作为合成氨基甲酸酯(甲基)丙烯酸酯低聚物时的催化剂,通常使用有机锡化合物。作为有机锡化合物,例如可以列举出:二月桂酸二丁基锡、二乙酸二丁基锡、马来酸二丁基锡、双(巯基乙酸2-乙基己酯)二丁基锡、双(巯基乙酸异辛酯)二丁基锡以及氧化二丁基锡。从易得性或催化性能的方面来看,优选使用二月桂酸二丁基锡或二乙酸二丁基锡作为催化剂。
在合成氨基甲酸酯(甲基)丙烯酸酯低聚物时也可以使用碳原子数为5以下的低级醇。作为低级醇,例如可以列举出:甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-2-丙醇、1-戊醇、2-戊醇、3-戊醇、2-甲基-1-丁醇、3-甲基-1-丁醇、2-甲基-2-丁醇、3-甲基-2-丁醇以及2,2-二甲基-1-丙醇。
本实施方式涉及的树脂组合物也可以进一步含有环氧(甲基)丙烯酸酯低聚物。作为环氧(甲基)丙烯酸酯低聚物,可以使用将具有(甲基)丙烯酰基的化合物与具有2个以上缩水甘油基的环氧树脂进行反应而得到的低聚物。
作为单体,可以使用具有1个可聚合基团的单官能单体、具有2个以上可聚合基团的多官能单体。单体也可以2种以上混合使用。
作为单官能单体,例如可以列举出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸仲丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸正戊酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸庚酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸2-苯氧基乙酯、丙烯酸3-苯氧基苄基酯、苯氧基二乙二醇丙烯酸酯、苯氧基聚乙二醇丙烯酸酯、丙烯酸4-叔丁基环己醇酯、(甲基)丙烯酸四氢糠酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸二环戊烯酯、(甲基)丙烯酸二环戊烯氧基乙酯、(甲基)丙烯酸二环戊酯、(甲基)丙烯酸壬基酚聚乙二醇酯、(甲基)丙烯酸壬基苯氧基聚乙二醇酯、(甲基)丙烯酸异冰片酯等(甲基)丙烯酸酯类单体;(甲基)丙烯酸、(甲基)丙烯酸二聚物、(甲基)丙烯酸羧基乙酯、(甲基)丙烯酸羧基戊酯、(甲基)丙烯酸ω-羧基-聚己内酯等含羧基的单体;N-丙烯酰基吗啉、N-乙烯基吡咯烷酮、N-乙烯基己内酰胺、N-丙烯酰基哌啶、N-甲基丙烯酰基哌啶、N-丙烯酰基吡咯烷、3-(3-吡啶基)丙基(甲基)丙烯酸酯、环三羟甲基丙烷甲缩醛丙烯酸酯等含杂环的(甲基)丙烯酸酯;马来酰亚胺、N-环己基马来酰亚胺、N-苯基马来酰亚胺等马来酰亚胺系单体;(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、N,N-二乙基(甲基)丙烯酰胺、N-己基(甲基)丙烯酰胺、N-甲基(甲基)丙烯酰胺、N-丁基(甲基)丙烯酰胺、N-丁基(甲基)丙烯酰胺、N-羟甲基(甲基)丙烯酰胺、N-羟甲基丙烷(甲基)丙烯酰胺等N-取代酰胺系单体;(甲基)丙烯酸氨基乙酯、(甲基)丙烯酸氨基丙酯、(甲基)丙烯酸N,N-二甲基氨基乙酯、(甲基)丙烯酸叔丁基氨基乙酯等(甲基)丙烯酸氨基烷基酯系单体;N-(甲基)丙烯酰氧基亚甲基琥珀酰亚胺、N-(甲基)丙烯酰基-6-氧基六亚甲基琥珀酰亚胺、N-(甲基)丙烯酰基-8-氧基八亚甲基琥珀酰亚胺等琥珀酰亚胺系单体。
作为多官能单体,例如可以列举出:乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯、双酚A的环氧烷加成物的二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、羟基新戊酸新戊二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、1,12-十二烷二醇二(甲基)丙烯酸酯、1,14-十四烷二醇二(甲基)丙烯酸酯、1,16-十六烷二醇二(甲基)丙烯酸酯、1,20-二十烷二醇二(甲基)丙烯酸酯、异戊二醇二(甲基)丙烯酸酯、3-乙基-1,8-辛二醇二(甲基)丙烯酸酯、双酚A的EO加成物二(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、三羟甲基辛烷三(甲基)丙烯酸酯、三羟甲基丙烷聚乙氧基三(甲基)丙烯酸酯、三羟甲基丙烷聚丙氧基三(甲基)丙烯酸酯、三羟甲基丙烷聚乙氧基聚丙氧基三(甲基)丙烯酸酯、三[(甲基)丙烯酰氧基乙基]异氰脲酸酯、季戊四醇三(甲基)丙烯酸酯、季戊四醇聚乙氧基四(甲基)丙烯酸酯、季戊四醇聚丙氧基四(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、二三羟甲基丙烷四(甲基)丙烯酸酯、二季戊四醇四(甲基)丙烯酸酯、二季戊四醇五(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯以及己内酯改性三[(甲基)丙烯酰氧基乙基]异氰脲酸酯。
作为光聚合引发剂,可以从公知的自由基光聚合引发剂当中适当地选择并使用。作为光聚合引发剂,例如可以列举出:1-羟基环己基苯基酮(Omnirad 184,IGM Resins公司制)、2,2-二甲氧基-2-苯基苯乙酮、1-(4-异丙基苯基)-2-羟基-2-甲基丙烷-1-酮、双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基戊基氧化膦、2-甲基-1-[4-(甲硫基)苯基]-2-吗啉基-丙烷-1-酮(Omnirad 907,IGM Resins公司制)、2,4,6-三甲基苯甲酰基二苯基氧化膦(Omnirad TPO,IGM Resins公司制)以及双(2,4,6-三甲基苯甲酰基)苯基氧化膦(Omnirad819,IGM Resins公司制)。
树脂组合物也可以进一步含有硅烷偶联剂、流平剂、消泡剂、抗氧化剂等。
作为硅烷偶联剂,只要其不妨碍树脂组合物的固化,则没有特别地限定。作为硅烷偶联剂,例如可以列举出:硅酸四甲酯、硅酸四乙酯、巯基丙基三甲氧基硅烷、乙烯基三氯硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基-乙氧基)硅烷、β-(3,4-环氧环己基)-乙基三甲氧基硅烷、二甲氧基二甲基硅烷、二乙氧基二甲基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基甲基二乙氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基三甲氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基三甲基二甲氧基硅烷、N-苯基-γ-氨基丙基三甲氧基硅烷、γ-氯丙基三甲氧基硅烷、γ-巯基丙基三甲氧基硅烷、γ-氨基丙基三甲氧基硅烷、双-[3-(三乙氧基甲硅烷基)丙基]四硫化物、双-[3-(三乙氧基甲硅烷基)丙基]二硫化物、γ-三甲氧基甲硅烷基丙基二甲基硫代氨甲酰基四硫化物以及γ-三甲氧基甲硅烷基丙基苯并噻唑基四硫化物。
本实施方式涉及的树脂组合物的粘度在45℃下优选为300mPa·s以上5000mPa·s以下、更优选为400mPa·s以上4500mPa·s以下、进一步优选为500mPa·s以上3500mPa·s以下、特别优选为700mPa·s以上3000mPa·s以下。通过使树脂组合物的粘度在上述范围内,可以提高树脂组合物的涂布性。
本实施方式涉及的树脂组合物可以适用于光纤的次级被覆材料。通过将本实施方式涉及的树脂组合物用于次级树脂层,可以制作出具有高杨氏模量和侧压特性优异的光纤。
<光纤>
图1是表示本实施方式涉及的光纤的一个例子的示意性剖面图。光纤10具备:含有芯部11和包层12的玻璃纤维13,以及设置在玻璃纤维13的外周且含有初级树脂层14和次级树脂层15的被覆树脂层16。
包层12包围着芯部11。芯部11和包层12主要包含石英玻璃等玻璃,例如,芯部11可以使用添加有锗的石英玻璃,包层12可以使用纯石英玻璃或添加有氟的石英玻璃。
在图1中,例如,玻璃纤维13的外径(D2)为125μm左右,构成玻璃纤维13的芯部11的直径(D1)为7~15μm左右。
被覆树脂层16的厚度通常为60~70μm左右。初级树脂层14和次级树脂层15的各层的厚度可以为10~50μm左右,例如,初级树脂层14的厚度可以为35μm,次级树脂层15的厚度可以为25μm。光纤10的外径可以为245~265μm左右。
另外,被覆树脂层16的厚度也可以为27~48μm左右。初级树脂层14和次级树脂层15的各层的厚度可以为10~38μm左右,例如,初级树脂层14的厚度可以为25μm,次级树脂层15的厚度可以为10μm。光纤10的外径可以为179~221μm左右。
进一步,玻璃纤维13的外径(D2)可以为100μm左右,被覆树脂层16的厚度可以为22~37μm左右。初级树脂层14和次级树脂层15的各层的厚度可以为5~32μm左右,例如,初级树脂层14的厚度可以为25μm,次级树脂层15的厚度可以为10μm。光纤10的外径可以为144~174μm左右。
本实施方式涉及的树脂组合物可以适用于次级树脂层。次级树脂层可以通过使包含上述基础树脂和表面修饰无机氧化物粒子的树脂组合物固化来形成。由此,能够提高光纤的侧压特性。
本实施方式涉及的光纤的制造方法包括:将上述树脂组合物涂布在由芯部和包层构成的玻璃纤维的外周的涂布工序;以及在涂布工序之后通过照射紫外线使树脂组合物固化的固化工序。
次级树脂层的杨氏模量在23℃下优选为1300MPa以上、更优选为1300MPa以上2600MPa以下、进一步优选为1500MPa以上2500MPa以下。当次级树脂层的杨氏模量为1300MPa以上时,容易提高侧压特性,当其为2600MPa以下时,能够对次级树脂层赋予适度的韧性,因而在次级树脂层中难以产生裂纹等。
分散在分散介质中的表面修饰无机氧化物粒子在树脂层固化后依然以分散的状态存在于树脂层中。在使用反应性的分散介质的情况下,表面修饰无机氧化物粒子与分散介质一起混合在树脂组合物中,并且在保持分散状态的情况下进入到树脂层中。在使用非反应性的分散介质的情况下,分散介质的至少一部分从树脂组合物中挥发并消失,但是表面修饰无机氧化物粒子依然以分散状态残留在树脂组合物中,并以分散的状态存在于固化后的树脂层中。在利用电子显微镜进行观察时,存在于树脂层中的表面修饰无机氧化物粒子以一次粒子分散的状态被观察到。
初级树脂层14例如可以是通过使包含氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂的树脂组合物固化而形成的。初级树脂层用的树脂组合物可以使用现有公知的技术。作为氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂,可以适当地选自上述基础树脂中所示例的化合物。但是,形成初级树脂层的树脂组合物与形成次级树脂层的基础树脂具有不同的组成。
需要说明的是,有时将多条光纤并列,并采用带用树脂一体化而成为光纤带,本发明的树脂组合物也可以用作带用树脂。由此,与光纤同样地,能够提高光纤带的侧压特性。
实施例
以下,示出了使用本发明涉及的实施例和比较例的评价试验结果并对本发明进行更详细的说明。需要说明的是,本发明不限于这些实施例。
[树脂组合物的制作]
(低聚物)
作为低聚物,准备了使分子量为600的聚丙二醇、2,4-甲苯二异氰酸酯、以及丙烯酸羟乙酯发生反应而得到的氨基甲酸酯丙烯酸酯低聚物,以及环氧丙烯酸酯低聚物。
(单体)
作为单体,准备了丙烯酸异冰片酯(“大阪有機化学工業株式会社”的商品名“IBXA”)、三丙二醇二丙烯酸酯(“ダイセル·オルネクス株式会社”的商品名“TPGDA”)以及丙烯酸2-苯氧基乙酯(“共栄化学株式会社”的商品名“ライトアクリレートPO-A”)。
(光聚合引发剂)
作为光聚合引发剂,准备了1-羟基环己基苯基酮和2,4,6-三甲基苯甲酰基二苯基氧化膦。
(基础树脂)
将45质量份的氨基甲酸酯丙烯酸酯低聚物、13.4质量份的环氧丙烯酸酯、9质量份的丙烯酸异冰片酯、22.5质量份的三丙二醇二丙烯酸酯、10质量份的丙烯酸2-苯氧基乙酯、0.05质量份的1-羟基环己基苯基酮、以及0.05质量份的2,4,6-三甲基苯甲酰基二苯基氧化膦混合,从而制备了基础树脂。
(表面修饰无机氧化物粒子)
作为表面修饰无机氧化物粒子,准备了含有通过对表1所示的化合物进行表面处理而得的氧化硅粒子(以下,简称“氧化硅粒子”)的氧化硅溶胶(MEK分散液)。
(实施例1~3、比较例1)
将基础树脂和氧化硅溶胶混合后,除去大部分的MEK,从而制备了树脂组合物,使得树脂组合物中的氧化硅粒子的含量成为表1所示的值。
(表面修饰量的测定)
在树脂组合物中加入氯仿后进行离心分离,回收沉淀物。在沉淀物中加入丙酮后进行离心分离,除去上清液后,在沉淀物中再次加入丙酮后进行离心分离并除去上清液,将上述操作进行4次,从而提取出氧化硅粒子。将用研钵捣碎后的氧化硅粒子在室温下减压干燥12小时以除去挥发性成分。在30000rpm、120分钟的条件下进行离心分离。将干燥后的氧化硅粒子在80℃下减压处理12小时,使用细孔分布测定装置(“マイクロメリティクス”制造的“ASAP-2020”),利用氮吸附BET法测定了氧化硅粒子的比表面积(m2/g)。
使用差热热重量同时分析装置(“日立ハイテクサイエンス”公司制造的“TG/DTA6300”)测定了氧化硅粒子中所含的有机成分的比例(质量%)。测定如下:将测定了重量后的氧化硅粒子在氮气下(300mL/分钟)从室温加热至850℃,然后从850℃冷却至200℃,再在空气下(100mL/分钟)从200℃加热至1000℃,测定重量变化。由氧化硅粒子的重量变化算出有机成分的比例。
根据氧化硅粒子的比表面积和有机成分的比例,通过下式算出氧化硅粒子的表面修饰量。
表面修饰量(mg/m2)=有机成分的比例/比表面积
(比较例2)
使用基础树脂作为树脂组合物。
使用实施例和比较例中所得到的树脂组合物进行了以下评价。结果如表1所示。比较例1的树脂组合物因氧化硅粒子的分散性差而无法进行评价。
(粘度)
使用B型粘度计(“ブルックフィ-ルド”公司制造的“数字式粘度计DV-II”、使用的主轴:No.18、转速:10rpm)测定了树脂组合物在45℃下的粘度。
(杨氏模量)
利用旋涂机,将实施例或比较例中所得的树脂组合物涂布在聚对苯二甲酸乙二醇酯(PET)膜上后,使用无电极UV灯系统(“ヘレウス”制造的“VPS600(D阀)”),在1000±100mJ/cm2的条件下使其固化,从而在PET膜上形成厚度为200±20μm的树脂层。将树脂层从PET膜上剥离,从而得到了树脂膜。
将树脂膜冲切成JIS K 7127 Type5的哑铃状,并在23±2℃、50±10%RH的条件下,使用拉伸试验机以1mm/分钟的拉伸速度、标线间隔25mm的条件下拉伸,从而得到应力-应变曲线。由2.5%切线求出杨氏模量。
[光纤的制作]
准备了通过使分子量为4000的聚丙二醇、异佛尔酮二异氰酸酯、丙烯酸羟乙酯以及甲醇发生反应而得到的氨基甲酸酯丙烯酸酯低聚物。将75质量份的氨基甲酸酯丙烯酸酯低聚物、12质量份的壬基苯酚EO改性丙烯酸酯、6质量份的N-乙烯基己内酰胺、2质量份的1,6-己二醇二丙烯酸酯、1质量份的2,4,6-三甲基苯甲酰基二苯基氧化膦以及1质量份的3-巯基丙基三甲氧基硅烷混合,从而得到了初级树脂层用的树脂组合物A1。
在由芯部和包层构成的直径为125μm的玻璃纤维的外周,将树脂组合物A1作为初级树脂层用、将实施例或比较例的树脂组合物作为次级树脂层用来进行涂布,然后通过照射紫外线使树脂组合物固化,形成厚度为35μm的初级树脂层和其外周的次级树脂层,从而制作了光纤。将线速度设为1500m/分钟。
(涂布性)
对于所制作的光纤,通过确认是否发生断线和树脂层是否产生裂纹来评价树脂组合物的涂布性。将没有发生断线、树脂层没有产生裂纹的情况设为“A”;将发生断线、但树脂层没有产生裂纹的情况设为“B”;将发生断线、树脂层产生裂纹的情况设为“C”。当树脂组合物的粘度过高时,形成次级树脂层时的被覆直径不稳定,容易发生断线。另一方面,当树脂组合物的粘度过低时,自对准力难以发挥作用,容易产生厚度偏差。
[表1]
可以确认:实施例的树脂组合物可以形成具有次级树脂层所需要的高杨氏模量、并且涂布性优异的强韧的树脂层。
符号说明
10…光纤、11…芯部、12…包层、13…玻璃纤维、14…初级树脂层、15…次级树脂层、16…被覆树脂层。
Claims (8)
1.一种光纤被覆用的树脂组合物,包括:
含有氨基甲酸酯(甲基)丙烯酸酯低聚物、单体以及光聚合引发剂的基础树脂;以及具有碳原子数为1以上8以下的烷基或苯基的表面修饰无机氧化物粒子,
以所述树脂组合物的总量为基准,所述表面修饰无机氧化物粒子的含量为1质量%以上60质量%以下,
所述表面修饰无机氧化物粒子中的表面修饰量为0.15mg/m2以上。
2.根据权利要求1所述的树脂组合物,其中,
所述表面修饰量为0.15mg/m2以上2.5mg/m2以下。
3.根据权利要求1或权利要求2所述的树脂组合物,其中,
所述烷基是选自由甲基、乙基、丙基、丁基、戊基、己基以及辛基构成的组中的至少1种基团。
4.根据权利要求1至权利要求3中任意一项所述的树脂组合物,其中,
所述表面修饰无机氧化物粒子的平均一次粒径为800nm以下。
5.根据权利要求1至权利要求4中任意一项所述的树脂组合物,其中,
粘度在45℃为300mPa·s以上5000mPa·s以下。
6.一种光纤的次级被覆材料,包括权利要求1至权利要求5中任意一项所述的树脂组合物。
7.一种光纤,具备:
含有芯部和包层的玻璃纤维、
与所述玻璃纤维接触并被覆该玻璃纤维的初级树脂层、以及被覆所述初级树脂层的次级树脂层,其中,
所述次级树脂层由权利要求1至权利要求5中任意一项所述的树脂组合物的固化产物构成。
8.一种光纤的制造方法,包括:
将权利要求1至权利要求5中任意一项所述的树脂组合物涂布在含有芯部和包层的玻璃纤维的外周的涂布工序;以及
在所述涂布工序之后通过照射紫外线使所述树脂组合物固化的固化工序。
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