CN116285441B - 一种用于光学晶体表面防潮抗污染减反膜及其制备方法 - Google Patents
一种用于光学晶体表面防潮抗污染减反膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于光学晶体表面防潮抗污染减反膜的制备方法,采用正硅酸乙酯为原料,采用溶胶‑凝胶法制备硅溶胶颗粒,然后以含氟硅氮烷为改性剂,对二氧化硅表面进行化学接枝,得到溶胶进行处理后对光学晶体表面镀膜得到减反膜,无需热处理。该减反膜表面有很低的自由能,表现出很高的疏水疏油性能,可以保证其本身与光学晶体在使用过程中不被污染物侵蚀,并在长时间使用过程中保持很高的透过率,并且该减反膜无需高温处理,拓宽了该减反膜的应用范围。
Description
技术领域
本发明涉及减反膜,特别涉及一种用于光学晶体表面防潮抗污染减反膜及其制备方法。
背景技术
溶胶凝胶法相对于其他制备减反膜的方法而言,具有成本低、工艺简单、成膜面积大、抗损伤阈值高等优点,被广泛的应用到高功率激光器件中。但由于此类膜层由大量纳米二氧化硅颗粒堆积而成,表面具有丰富的微孔结构和残余的硅羟基,容易吸附空气中的水和有机物质,造成膜层光学性能下降,尤其对于磷酸二氢钾(KDP)或磷酸二氘钾(DKDP)等水溶性晶体而言,水的侵蚀会对光滑的光学表面造成不可逆的损伤。目前对溶胶凝胶法制备光学薄膜的改进主要有以下几种:气氛处理、添加疏水物质、增镀保护层和硅溶胶表面改性。其中气氛处理的方法在过程中会引入或产生小分子杂质,可能会对光学晶体产生不可逆损伤,并且部分需高温加热;添加疏水物质和增镀保护层的方法,会使得膜层孔隙率发生改变,从而改变膜层折射率进而影响膜层透过率,并且需要后续高温热处理(>120℃)使膜层稳定。2014年ZHANG Qing-Hua等人在Journal of Inorganic Materials 29(2014)667-672一文中,通过碱催化正硅酸乙酯反应,加入20氟基-1,12-十二醇控制二氧化硅颗粒的结构和尺寸,并加入甲基丙烯酸六氟丁酯的聚合物(PHFBMA)作为填充剂对膜层孔隙进行填充,旋涂后160℃热处理24h得到耐真空污染的增透膜,该方法通过添加含氟小分子和聚合物,使得膜层表面能降低,实现抗真空污染的目的,但填充物与硅溶胶之间无化学键合,仍需高温处理。对于上述方法,不适用于部分相转变温度较低的光学晶体,如DKDP晶体的相转变温度仅为120℃左右,当热处理温度为110-120℃时,会使得氘代晶体完全破坏,这限制了此类方法的应用。
硅溶胶表面化学改性是一种简单有效的方式,通过一步法或一锅法,在溶胶阶段对二氧化硅颗粒表面进行化学接枝,通过共价结合的方式对其进行改性,后续不需对膜层进行高温热处理,即可得到性能良好的减反膜。2003年Suratwala等人在Journal of Non-Crystalline Solids 316(2003)349–363中提出在溶胶制备结束后,将六甲基二硅胺烷引入溶胶中进行化学改性,得到的膜层膜层的疏水防潮性能获得极大提高,并且后续研究中证明该方法的抗真空污染性能也有很大提高。含氟材料本身具有极低的表面能,具有良好的疏水疏油性能,通过化学接枝将氟基团引入减反膜中,可以增强减反膜的抗真空污染性能。中国发明专利201811307553.6公开了一种采用酸催化硅酸四乙酯聚合,并在酸催化下加入改性剂2,2,3,3,4,4,5,5,6,6,7,7-全氟-1,8-辛二醇对硅溶胶表面进行化学接枝,添加聚六氟-2-甲基异丙基丙烯酸酯作为填充剂,从而实现真空装置中膜层的高透过率。采用酸催化的方式,硅酸四乙酯酸性水解更容易形成线性聚合物,从而使得成膜后孔隙率降低折射率升高,不利于膜层应用。
发明内容
本发明的目的在于针对现有技术的不足之处,本发明通过采用碱催化硅酸四乙酯反应制备硅溶胶,一锅法加入小分子含氟硅氮烷与二氧化硅颗粒表面硅羟基反应,反应结束后通过蒸馏除去杂质即可得到减反膜所用硅溶胶,通过提拉法或旋涂法镀膜后,无需高温热处理,即可得到性能优异的减反膜。该方法通过化学接枝得到氟改性硅溶胶,具有更好的稳定性与更低的表面能,具有优异的疏水疏油效果。并且溶胶通过一锅碱催化法制备,使得减反膜具有更低的折射率,大大扩大了后期应用范围。
本发明提供一种低温下制备防潮抗污染减反膜的制备方法制备方法,包括:将硅酸四乙酯、氨水和乙醇混合,得到溶胶A,陈化一定时间后,加入小分子含氟硅氮烷的溶液混合陈化后得到氟改性的硅溶胶B,真空蒸馏除去低沸点杂质后得到目标溶胶C,使用溶胶C旋涂或提拉法制得防潮抗污染减反膜。
本发明通过采用小分子含氟硅氮烷与二氧化硅表面羟基进行反应,在不改变二氧化硅颗粒大小的情况下通过化学接枝使二氧化硅颗粒表面富含氟基,不改变膜层结构,成膜后膜层折射率不增大,从而保证膜层减反增透效果不受影响。具体表现为:膜层本身具有优良的疏水疏油效果,在含水蒸气与挥发性有机物换进中不容易吸附吸附污染物并且长期保持很高的透过率。
进一步地,在本发明较佳实施例中,上述制备方法包括以下步骤:
(1)将硅酸四乙酯、氨水和乙醇按照(2.5-4):(0.5-1.5):(20-40)的质量比在一定温度下搅拌混合,在一定温度下陈化7天,得到溶胶A;
(2)将含氟硅氮烷溶解在溶剂中,按照含氟硅氮烷与硅酸四乙酯摩尔比0.75-1.5的比例,加入溶胶A中并混合均匀,在一定温度下陈化得到溶胶B;
(3)将溶胶B在一定条件下真空蒸馏除去杂质后,得到溶胶C,即最终溶胶;
(4)使用溶胶C以旋涂或提拉法涂覆在基片表面,得到防潮抗污染减反膜,在指定波长透过率大于99%。
进一步的,根据本发明优选的,步骤(1)中,硅酸四乙酯、氨水、水和乙醇的混合温度为5-8℃,搅拌时间为2-6小时。
进一步的,根据本发明优选的,步骤(2)中溶解含氟硅氮烷为1,3-双(3,3,3-三氟丙基)-1,1,3,3-四甲基二硅氮烷、1,3-二五氟苯基苯基四甲基二硅氮烷、双全氟辛基四甲基二硅氮烷中的一种或几种组合
进一步的,根据本发明优选的,步骤(2)中溶解含氟硅氮烷的溶剂为二甲苯、乙苯、正辛烷、正癸烷、壬烷、全氟己烷、全氟环己烷、全氟甲基环己烷、全氟甲苯、全氟庚烷中的一种或几种的组合。
进一步的,根据本发明优选的,步骤(2)中陈化温度为15-25℃,陈化时间为7-21天。
进一步的,根据本发明优选的,步骤(3)中真空蒸馏的真空度为-0.08~-0.1MPa,温度为40-70℃。
本发明所得防潮抗污染减反膜具有良好的抗湿气和有机污染物性能,在1064nm或532nm波段具有大于99.5的透过率,激光抗损伤阈值可达到30J/cm2左右,并且在污染环境中放置30天后相应波长下透过率仅有略微下降。
附图说明
图1为实施例1中制得减反膜的扫描电镜照片;
图2为实施例1中制得减反膜的疏水角照片;
图3为实施例1中制得减反膜的疏油角(甲苯)照片;
图4为实施例1中磷酸二氘钾基底与制得减反膜在甲苯溶剂环境中放置30天的透过率变化曲线对比图
具体实施方式
实施例1
取208g硅酸四乙酯、58g氨水、2g水和1800g无水乙醇混合,在20℃下搅拌4小时,使其混合均匀,在20℃下陈化7天,得到溶胶A;取325g 1,3-双(3,3,3-三氟丙基)-1,1,3,3-四甲基二硅氮烷与500g二甲苯和500g八氟甲苯加入溶胶A中,搅拌2h混合均匀,20℃陈化14天得到溶胶B;在-0.1Mpa,40摄氏度水浴真空蒸馏除去体系中乙醇、水等杂质,得到溶胶C,溶胶颗粒直径为25nm;采用400rpm/min的旋涂速度将溶胶涂覆在清洁后的磷酸二氘钾基片上,得到厚度为220nm的膜层,在1064nm透过率为99.9%,抗损伤阈值为31J/cm2(10ns,1064nm),疏水角为137°,疏油角为113°(甲苯),在25℃,在25℃,甲苯气氛中静置30天,1064nm透过率下降为99.6%。
实施例2
取硅酸四乙酯312g、氨水60g和无水乙醇1800g混合,在20℃下搅拌4小时,使其混合均匀,在20℃下陈化7天,得到溶胶A;取325g 1,3-双(3,3,3-三氟丙基)-1,1,3,3-四甲基二硅氮烷、1000g壬烷与200g全氟己烷加入溶胶A中,搅拌2h混合均匀,20℃陈化14天得到溶胶B;在-0.1Mpa,50℃水浴真空蒸馏除去体系中乙醇、水等杂质,得到溶胶C,溶胶颗粒直径为20nm;采用800rpm/min的旋涂速度将溶胶涂覆在清洁后的基片上,得到厚度为110nm的膜层,在532nm透过率为99.6%。抗损伤阈值为29J/cm2(10ns,1064nm)。
本技术领域技术人员可以理解,除非另外定义,这里使用的所有术语(包括技术术语和科学术语),具有与本发明所属领域中的普通技术人员的一般理解相同的意义。还应该理解的是,诸如通用字典中定义的那些术语,应该被理解为具有与现有技术的上下文中的意义一致的意义,并且除非像这里一样被特定定义,否则不会用理想化或过于正式的含义来解释。
应当理解,以上借助优选实施例对本发明的技术方案进行的详细说明是示意性的而非限制性的。本领域的普通技术人员在阅读本发明说明书的基础上可以对各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (6)
1.一种光学晶体表面防潮抗污染减反膜的制备方法,其特征在于,所述制备方法包括以下步骤:
(1)将硅酸四乙酯、氨水和和乙醇按照(2.5-4):(0.5-1.5):(20-40)的质量比搅拌混合,在一定温度下陈化,得到溶胶A;
(2)将含氟硅氮烷溶解在溶剂中,按照含氟硅氮烷与硅酸四乙酯摩尔比0.75-1.5的比例,加入溶胶A中并混合均匀,在一定温度下陈化得到溶胶B;
(3)将溶胶B真空蒸馏,得到溶胶C,即最终溶胶;
(4)使用溶胶C涂覆在基片表面,得到防潮抗污染减反膜;
步骤(2)中所述含氟硅氮烷为1,3-双(3,3,3-三氟丙基)-1,1,3,3-四甲基二硅氮烷、1,3-二五氟苯基苯基四甲基二硅氮烷、双全氟辛基四甲基二硅氮烷中的一种或几种组合。
2.根据权利要求1所述一种光学晶体表面防潮抗污染减反膜的制备方法,其特征在于,步骤(1)中硅酸四乙酯、氨水、水和乙醇的混合温度为5-8℃,搅拌时间为2-6小时。
3.根据权利要求1所述一种光学晶体表面防潮抗污染减反膜的制备方法,其特征在于,步骤(2)中所述溶剂为二甲苯、乙苯、正辛烷、正癸烷、壬烷、全氟己烷、全氟环己烷、全氟甲基环己烷、全氟甲苯、全氟庚烷中的一种或几种的组合。
4.根据权利要求1所述一种光学晶体表面防潮抗污染减反膜的制备方法,其特征在于,步骤(2)中在5-15℃,机械搅拌24-48小时混合均匀,陈化温度为15-20℃,陈化时间7-21天;和/或步骤(1)陈化时间7-21天。
5. 根据权利要求1所述一种光学晶体表面防潮抗污染减反膜的制备方法,其特征在于,步骤(3)中真空蒸馏的真空度为-0.08~-0.1 MPa,温度为40-70℃。
6.根据权利要求1所述一种光学晶体表面防潮抗污染减反膜的制备方法,其特征在于,步骤(4)中300-900rpm/min的旋涂速度。
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CN103771727A (zh) * | 2013-12-31 | 2014-05-07 | 河南安彩高科股份有限公司 | 减反射玻璃基板及其制法和用途 |
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CN103757706A (zh) * | 2014-01-08 | 2014-04-30 | 同济大学 | 一种非线性光学晶体表面增透保护膜的制备方法 |
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