溶胶-凝胶法制备抗激光损伤SiO<sub>2</sub>疏水减反射膜

徐耀; 范文浩; 黄祖鑫; 章斌; 吴东; 蒋晓东; 孙予罕; 魏晓峰

强激光与粒子束, 2004, 16 (1): 40, 网络出版: 2006-05-15

溶胶-凝胶法制备抗激光损伤SiO₂疏水减反射膜

Preparation of hydrophobic anti-reflective SiO₂ films for high laser resistance by Sol-Gel Process

论文大纲

徐耀 ¹范文浩 ¹黄祖鑫 ²章斌 ¹吴东 ¹蒋晓东 ²孙予罕 ¹魏晓峰 ²

作者单位

¹ 中国科学院,山西煤炭化学研究所,煤转化国家重点实验室,山西,太原,030001

² 中国工程物理研究院,激光聚变研究中心,四川,绵阳,621900

溶胶-凝胶疏水性减反射膜二氧化硅激光损伤 Sol-gel Hydrophobic Anti-reflectiv film Silica Laser damage

摘要

通过溶胶-凝胶法,在碱性条件下水解缩聚正硅酸乙酯获得含有SiO₂颗粒的溶胶;以甲基三乙氧基硅烷在酸性条件下水解缩聚获得双链聚合物溶液,作为疏水基团的引入剂.用两者的混合物在玻璃片上旋转镀膜.利用光子相干光谱法、透射电子显微镜、小角X射线散射等方法研究了溶胶微结构,利用紫外-可见光谱仪和接触角测定仪测量薄膜的透射率和疏水性.单面反射率最低降至0.01%,对水接触角最高为118°.利用Nd:YAG激光(1 064nm)测量了薄膜的激光损伤阈值,随混合溶胶中双链聚合物含量的增加损伤阈值减小,但均高于20J/cm²(1ns脉冲).由于薄膜既保持了纳米氧化硅薄膜的多孔性,又在颗粒及孔表面以甲基修饰,水对薄膜的浸润能力大大降低,因此薄膜的时间稳定性大大增强,同时也保证了较高的损伤阈值和透射率.

Abstract

A sol containing SiO₂ particles was prepared by the base catalyzed hydrolysis and polycondensation of tetraethoxysilane (TEOS) through sol-gel process. A solution containing double-chain polymer of methyltriethoxysilane (MTES) was also prepared under acid condition, as the introducer of water repellence. After mixing these two kinds of sols, spinning coating was used to deposit films on glass. Several techniquesphoton correlation spectrum,TEM and small angle X-ray scattering, were used to characterize the microstructure. The transmission and wet-angle for water of films were measured by UV-Vis and contact angle analyzer. The reflection can be reduced to 0.01% and the wet-angle for water was 118°at most. A Nd:YAG laser was used to determine the laser damage threshold of film at 1 064nm. The threshold decreased with the increasing content of double-chain polymer solution in sol mixture. But all the thresholds were higher than 20J/cm². Due to reserving porosity of nano-silica film and modifying the surface of pores by methyls , the wetting of water vapour to film weakened largely. The endurance of film improved , and high transmission and threshold were maintained.

参考文献

[1] Sto ?ber W,Fink.A,Bohn.E.Controlled growth of monodisperse silica spheres in the micro size range[J].JColloid Interface Sci,1968,26:62-66.

[2] Minami T,Katata N,Tadanaga K.Preparation and characterization of super-water-repellent Al₂O₃ coating films with high transparency[A].Bruce S Dunn SPIE V3136[C].1997.168-175.

[3] Nakagawa T,Soga M.A new method for fabricating water repellent silica films having high heat-resistance using the sol-gel method[J].J Non-Cryst Solids,1999,260:167-174.

[4] Hong B S,Han J H,Kim S T,et al.Endurable water-repellent glass for autobiles[J].Thin Solid Films,1999,351:274-278.

[5] Nakajima A,Abe K,Hashimoto K,et al.Preparation of hard super-hydrophobic films with visible light transmission[J].Thin Solid Films,2000,376:140-143.

[6] Tadanaga K,Morinaga J,Matsuada A,et al.Superhydrophobic-superhydrophilic micropatterning on flowerlike alumina coating film by the sol-gel method[J].Chem Mater,2000,12:590-592.

[7] Ogawa K,Soga M,Takada Y,et al.Development of a transparent and ultrahydrophobic glass plates[J].Jpn J Appl Phys,1993,32[4B]:614-615.

[8] Aksmatsu Y,Makita K ,Inaba H,et al.Water-repellent coating films on glass prepared from hydrolysis and polycondensation reactions of fluoroalkyltrialkoxylsilane[J].Thin Solid Films,2001,389:138-145.

[9] Brinker C J,Scherer G W.Sol-Gel Science[M].New York:Academic Press,1990.108-120.

[10] Zhang Z Y, Wakabayashi H.Structural study of Al(acac)₃ catalyzed CH₃SiO_1/2 gel[J].J of Sol-Gel Sci &Tech,1998,12:153-158.

[11] Capozzi C J,Pye L D,Sr Condrate R A.Vibrational spectral/structural changes from the hydrolysis/polycondensation of methyl-modified silicates[J].Mater Lett,1992,15:130-136.

[12] Wada M,Kamiya K,Nasu H.X-ay diffraction analysis of SiO₂ gel prepared from monomethyl-tri-ethoxysilane by the sol-gel method[J].Phys And Chem of Glasses,1992,33(2):56-60.

[13] Sakka S,Tanaka Y,Kokubo T.Hydrolysis and polycondensation of dimethyldiethoxysilane and methyltriethoxysilane as materials for the sol-gel process[J].J of non-Cryst Solids,1986,82:24-30.

[14] Yoldas B E,Partlow D B.Wide spectrum antireflection coating for fused silica and other glasses[J].Appl Opt,1984,23:1418-1422.

[15] Yoldas B E.Investigation of porous oxides an antireflective coating for glass surfaces[J].Appl Opt,1980,19:1425-1427.

[16] 王力衡,黄运添.薄膜技术(第一版)[M].北京:清华大学出版社,1991.119-126.
Wang L H,Huang Y T.Technology of thin films[M].Beijing:Tingshua University Press,1991.119-126.

[17] Milam D.Laser-induced damage at 1064nm 125psec[J].Appl Opt,1977,16(5):1204-1213.

[18] Strekalow V N.Absorption of laser light by ions as a mechanism of optical damage in solids[A].SPIE[C].1998,3244:26-31.

[19] Fornier A,Cordillot C,Bernardine D,et al.Towards the megajoule laser components[A].SPIE[C].1998,3244:64-75.

[20] Chow R.,Taylor J.R.,Wu Z.L.,et al.Absorption measurement of optical coatings-a round robin[A].SPIE[C].2001,4347:62-73.

徐耀, 范文浩, 黄祖鑫, 章斌, 吴东, 蒋晓东, 孙予罕, 魏晓峰. 溶胶-凝胶法制备抗激光损伤SiO₂疏水减反射膜[J]. 强激光与粒子束, 2004, 16(1): 40. XU Yao, FAN Wen-hao, HUANG Zu-xin, ZHANG Bin, WU Dong, JIANG Xiao-dong, SUN Yu-han, WEI Xiao-feng. Preparation of hydrophobic anti-reflective SiO₂ films for high laser resistance by Sol-Gel Process[J]. High Power Laser and Particle Beams, 2004, 16(1): 40.

溶胶-凝胶法制备抗激光损伤SiO₂疏水减反射膜

关于本站 Cookie 的使用提示

全站搜索

溶胶-凝胶法制备抗激光损伤SiO2疏水减反射膜

相关论文

相关资讯

关于本站 Cookie 的使用提示

全站搜索

溶胶-凝胶法制备抗激光损伤SiO₂疏水减反射膜