NH_3/HTMS气相法改性SiO_2增透膜的耐环境稳定性
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摘要
溶胶-凝胶法制备的二氧化硅增透膜因具有极低的折射率与较高的激光损伤阈值而被广泛应用于高功率激光系统中。但是,激光系统工作环境中的水汽及挥发性有机污染物极易污染薄膜。本研究以正硅酸四乙酯为前驱体,氨水为催化剂,乙醇为溶剂制备了碱性催化的单分散SiO_2溶胶。采用提拉法在BK7玻璃基板表面镀制了SiO_2薄膜,并对薄膜进行氨水气氛以及HTMS气氛联合处理改性。改性后的薄膜表现出了极佳的耐环境稳定性,在高湿环境下放置2个月后膜层峰值透过率仅下降0.03%,在低真空二甲基硅油污染环境下放置2个月后透过率光谱几乎无变化。NH_3/HTMS气相法联合处理可以有效延长SiO_2增透膜在高功率激光系统中的工作寿命。
Sol-Gel derived silica antireflective coatings have been widely used in high power laser system because of their ultra-low refractive index and high laser damage threshold. However, water vapor and volatile organic compounds in the laser system contaminate these coatings and reduce their antireflective efficiency and laser damage resistance. In this work, environmental stable SiO_2 antireflective coating was prepared by vapor phase treatment of ammonia and HTMS. Monodisperse colloidal silica sol was synthesized by Sol-Gel method using tetraethylorthosilicate(TEOS) as precursor, ammonia as catalyst, and ethanol as solvent. The silica coatings were then deposited on the BK7 glass using dip-coating method. Ammonia vapor phase treatment and HTMS vapor phase treatment were combined to improve the environmental stability of the antireflective coating. The peak transmittance of the BK7 glass coated with the modified coating decreased only 0.03% after being exposed in the humid environment for 2 m. Meanwhile, the transmittance curve of the BK7 glass coated with modified coating had almost no change after being placed under low vacuum condition with oil pollutants for 2 m, indicating that the coating modified via combined vapor phase treatment of ammonia and HTMS possessed an excellent environmental stable performance. Therefore, the combination of ammonia and HTMS vapor phase treatment is effective to improve the working life of SiO_2 antireflective coating in high power laser system.
Sol-Gel derived silica antireflective coatings have been widely used in high power laser system because of their ultra-low refractive index and high laser damage threshold. However, water vapor and volatile organic compounds in the laser system contaminate these coatings and reduce their antireflective efficiency and laser damage resistance. In this work, environmental stable SiO_2 antireflective coating was prepared by vapor phase treatment of ammonia and HTMS. Monodisperse colloidal silica sol was synthesized by Sol-Gel method using tetraethylorthosilicate(TEOS) as precursor, ammonia as catalyst, and ethanol as solvent. The silica coatings were then deposited on the BK7 glass using dip-coating method. Ammonia vapor phase treatment and HTMS vapor phase treatment were combined to improve the environmental stability of the antireflective coating. The peak transmittance of the BK7 glass coated with the modified coating decreased only 0.03% after being exposed in the humid environment for 2 m. Meanwhile, the transmittance curve of the BK7 glass coated with modified coating had almost no change after being placed under low vacuum condition with oil pollutants for 2 m, indicating that the coating modified via combined vapor phase treatment of ammonia and HTMS possessed an excellent environmental stable performance. Therefore, the combination of ammonia and HTMS vapor phase treatment is effective to improve the working life of SiO_2 antireflective coating in high power laser system.
引文
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[23]SUN JING-HUA,ZHANG QING-HUA,DING RUI-MIN,et al.Contamination-resistant silica antireflective coating with closed ordered mesopores.Physical Chemistry Chemical Physic,2014,16(31):16684-16693.
[24]SUN JING-HUA,ZHANG CE,ZHANG CONG,et al.Effect of post-treatment on ordered mesoporous silica antireflective coating.RSC Advances,2014,4(92):50873-50881.
[25]SUN JING-HUA,CUI XIN-MIN,ZHANG CE,et al.A broadband antireflective coating based on a double-layer system containing mesoporous silica and nanoporous silica.Journal of Materials Chemistry,2015,3(27):7187-7194.
[26]HUO YAN-FANG,LUO RONG-HUI,SU YONG-GANG.Comparison of base-catalyzed silica antireflective coatings modification by different surface treatments of water-NH3 and/or hexamethyldisilazane vapors.Acta Photonica Sinica,2013,42(7):823-827.
[27]SHEN JUN,LIU YUAN,LI XIAO-GUANG.Surface modification and contamination resistantce of Sol-Gel Si O2 derived antireflective coatings.Journal of the Chinese Ceramic Society,2010,38(11):2054-2058.
[28]LI XIAO-GUANG,SHEN JUN.The stability of Sol-Gel silica coatings in vacuum with organic contaminants.Journal of Sol-Gel Science and Technology,2011,59(3):539-545.
[29]VOORHEES P W.The theory of Ostwald ripening.Journal of Statistical Physics,1985,38(1/2):231-252.
[30]ZHANG XIN-XIANG,SU WEN-MU,LIN MING-YUE,et al.Non-supercritical drying Sol-Gel preparation of superhydrophobic aerogel ORMOSIL thin films with controlled refractive index.Journal of Sol-Gel Science and Technology,2015,74(3):594-602.
[31]RUI M,ALMEIDA,PANTANO CARL G.Structural investigation of silica gel films by infrared spectroscopy.Journal of Applied Physics,1990,68(8):4225-4232.
[32]GONCALVES GIL,MARQUES PAULA A A P,PINTORICARDO J B,et al.Surface modification of cellulosic fibres for multi-purpose TiO2 based nanocomposites.Composites Science and Technology,2009,69(7/8):1051-1056.
[33]MACLEOD H,ANGUS.Thin-film Optical Filters.Fourth Edition.Tucsou,Arizona,USA:Thin Film Center Incorporated,2010,106-112.
[2]WU GUANG-MING,SHEN JUN,WU YU,et al.Strengthening investigation of anti-reflective nano-porous silica films derived by base/acid two-step Sol-Gel process and mixed atmosphere treatment.Atomic Energy Science and Technology,2002,36(z1):374-379.
[3]ST?BER WERNER,FINK ARTHUR,BOHN ERNST.Controlled growth of monodisperse silica spheres in the micron size range.Journal of Colloid and Interface Science,1968,26(1):62-69.
[4]WANG XIAO-DONG,SHEN JUN.A review of contaminationresistant antireflective Sol-Gel coatings.Journal of Sol-Gel Science and Technology,2012,61(1):206-212.
[5]ZHANG QING-HUA,ZHOU LIAN,YANG WEI,et al.Sol-Gel preparation of a silica antireflective coating with enhanced hydrophobicity and optical stability in vacuum.Chinese Optics Letters,2014,12(7):071601-1-4.
[6]ZHANG XIN-XIANG,ZHUANG MENG-YUN,MIAO XIA,et al.Environment-resistant fluoro-containing antireflective coatings for high-powered laser systems.RSC Advances,2014,4(90):48872-48875.
[7]ZHANG XIN-XIANG,LIN MING-YUE,LIN LI-XIAO,et al.Sol-Gel preparation of fluoro-containing ORMOSIL antireflective coating with resistance simultaneously to hydrophilic and oleophilic pollutants.Journal of Sol-Gel Science and Technology,2015,74(3):698-706.
[8]ZHANG QING-HUA,WEI YAO-WEI,YANG WEI,et al.Improvement on contamination resistance to volatile organics and moisture of Sol-Gel silica antireflective coating for 351 nm laser system by structural modulation with fluorinated compounds.RSCAdvances,2014,5(6):4529-4536.
[9]YAN LIANG-HONG,CHI FANG-TING,JIANG XIAO-DONG,et al.Preparation of hydro-oleophobic silica antireflective coating.Journal of Inorganic Materials,2007,22(6):1247-1250.
[10]NIU YAN-YAN,WANG XIAO-DONG,YAO LAN-FANG,et al.Preparation of octyltrimethoxysilane modified SiO2 hydrophobic antireflective coating.Journal of Inorganic Materials,2016,31(5):499-504.
[11]LI HAI-YUAN,TANG YONG-XING.Study on stability of porous silica antireflective coatings prepared by Sol-Gel processing dash with organic silica.Chinese Journal of Lasers,2006,33(1):116-119.
[12]ZHANG YU-LU,ZHANG XIN-XIANG,YE HAI-PING,et al.Asimple route to prepare crack-free thick antireflective silica coatings with improved antireflective stability.Materials Letters,2012,69(4):86-88.
[13]ZHANG XIN-XIANG,XIA BI-BO,YE HAI-PING,et al.One-step Sol-Gel preparation of PDMS-silica ORMOSILs as environmentresistant and crack-free thick antireflective coatings.Journal of Materials Chemistry,2012,22(26):13132-13140.
[14]ZHANG XIN-XIANG,ZHENG FENG,YE LONG-QIANG,et al.A one-pot Sol-Gel process to prepare a superhydrophobic and environment-resistant thin film from ORMOSIL nanoparticles.RSC Advances,2014,4(19):9838-9841.
[15]YUAN Y,YAN G H,HUANG S H,et al.Preparation of hydrophobic SiO2/PMHS sol and ORMOSIL antireflective films for solar glass cover.Solar Energy,2016,130:1-9.
[16]YUAN YE,YAN GENG-HUA,LIU SHAO-ZHE,et al.Hydrophobic,ultra-low refractive index films prepared by Sol-Gel process.Materials Letters,2016,184:305-307.
[17]TAO CHAO-YOU,YAN HONG-WEI,YUAN XIAO-DONG,et al.Detailed analysis and formation mechanism of superhydrophobic antireflective coatings with adjustable refractive index from trimethylsilanized silica nanoparticles.Journal of Sol-Gel Science and Technology,2016,80(1):1-9.
[18]LIU YUAN,SHEN JUN,ZHOU BIN,et al.Effect of hydrophobicity on the stability of Sol-Gel silica coatings in vacuum and their laser damage threshold.Journal of Sol-Gel Science and Technology,2013,68(1):81-87.
[19]ZHANG XIN-XIANG,CAO CONG-RUI,XIAO BO,et al.Preparation and characterization of polyvinyl butyral/silica hybrid antireflective coating:effect of PVB on moisture-resistance and hydrophobicity.Journal of Sol-Gel Science and Technology,2010,53(1):79-84.
[20]XIAO BO,ZHANG YU-LU,ZHANG XIN-XIANG,et al.Focus on moisture-resistance and hydrophobicity of SiO2 antireflective film improved by poly(isopropylene oxide)glycerolether.Journal of Sol-Gel Science and Technology,2011,60(1):11-16.
[21]MARSHALL K L,ASHE B,RIGATTI A L,et al.Vaporphase-deposited organosilane coatings as hardening agents for high-peak-power laser optics.Proceedings of SPIE-The International Society for Optical Engineering,2007,6674:667407-1-11.
[22]WU BAO-HU,WU DONG,JIA HONG-BAO,et al.Fluoroalkylgrafted mesoporous silica antireflective films with enhanced stability in vacuum.Optics Letters,2012,37(19):4095-4097.
[23]SUN JING-HUA,ZHANG QING-HUA,DING RUI-MIN,et al.Contamination-resistant silica antireflective coating with closed ordered mesopores.Physical Chemistry Chemical Physic,2014,16(31):16684-16693.
[24]SUN JING-HUA,ZHANG CE,ZHANG CONG,et al.Effect of post-treatment on ordered mesoporous silica antireflective coating.RSC Advances,2014,4(92):50873-50881.
[25]SUN JING-HUA,CUI XIN-MIN,ZHANG CE,et al.A broadband antireflective coating based on a double-layer system containing mesoporous silica and nanoporous silica.Journal of Materials Chemistry,2015,3(27):7187-7194.
[26]HUO YAN-FANG,LUO RONG-HUI,SU YONG-GANG.Comparison of base-catalyzed silica antireflective coatings modification by different surface treatments of water-NH3 and/or hexamethyldisilazane vapors.Acta Photonica Sinica,2013,42(7):823-827.
[27]SHEN JUN,LIU YUAN,LI XIAO-GUANG.Surface modification and contamination resistantce of Sol-Gel Si O2 derived antireflective coatings.Journal of the Chinese Ceramic Society,2010,38(11):2054-2058.
[28]LI XIAO-GUANG,SHEN JUN.The stability of Sol-Gel silica coatings in vacuum with organic contaminants.Journal of Sol-Gel Science and Technology,2011,59(3):539-545.
[29]VOORHEES P W.The theory of Ostwald ripening.Journal of Statistical Physics,1985,38(1/2):231-252.
[30]ZHANG XIN-XIANG,SU WEN-MU,LIN MING-YUE,et al.Non-supercritical drying Sol-Gel preparation of superhydrophobic aerogel ORMOSIL thin films with controlled refractive index.Journal of Sol-Gel Science and Technology,2015,74(3):594-602.
[31]RUI M,ALMEIDA,PANTANO CARL G.Structural investigation of silica gel films by infrared spectroscopy.Journal of Applied Physics,1990,68(8):4225-4232.
[32]GONCALVES GIL,MARQUES PAULA A A P,PINTORICARDO J B,et al.Surface modification of cellulosic fibres for multi-purpose TiO2 based nanocomposites.Composites Science and Technology,2009,69(7/8):1051-1056.
[33]MACLEOD H,ANGUS.Thin-film Optical Filters.Fourth Edition.Tucsou,Arizona,USA:Thin Film Center Incorporated,2010,106-112.