Study on the Preparation and Properties of Novel Silica Microporous Antireflective Coating by Sol-Gel Process
SHANG Meng-ying1, 2, 3, CAO Lin-hong2, 3, LIU Miao1, LUO Xuan1, REN Hong-bo1, YE Xin1, TANG Yong-jian1, JIANG Xiao-dong1*
1. Research Center of Laser Fusion，China Academy of Engineering Physics，Mianyang 621900，China 2. State Key Laboratory Cultivation Base for Nonmetal Composites and Functional Materials，Department of Materials Science and Engineering, Southwest University of Science and Technology，Mianyang 621010，China 3. Laboratory for Extreme Conditions Matter Properties，Department of Materials Science and Engineering，Southwest University of Science and Technology, Mianyang 621010，China
Abstract：Silica sol was prepared by acid catalyzed sol-gel process using tetraethylorthosilicate (TEOS) as precursor and dimethyldietoxysilane (DDS) as pore-forming agent. A novel kind of monolayer microporous silica anti-reflective (AR) coating was obtained on K9 glass substrate by dip-coating technique and then heat treated at 500 ℃. The effects of different DDS/TEOS molar ratios on refractive index，transmittance and hardness were investigated. A positive correlation was found between the transmittance and the DDS/TEOS molar ratio due to the increasing porosity. The maximum transmittance can reach 99.7％ with the molar ratio of DDS/TEOS rising to 1∶1. Meanwhile，the refractive index was found quite close to the ideal value 1.22. Nevertheless，higher molar ratio will lead to a bad film-forming property. On the other hand，the hardness of the coatings decreased with the DDS increasing but still remained more than 2 h when the transmittance reached highest. Besides，these coatings exhibit a well abrasion-resistance and excellent adhesivity. The maximum transmittance was only dropped by 0.071% and 0.112% after abrasion for 500 and 1 000 times respectively. Accelerated corrosion tests indicated that the transmittance of traditional coatings rapidly fell down to the substrate level (～92%) after immersion for 5 min，while the transmittance of our novel coating almost linearly decreased and was kept 93.2% after 56 min. In other words，the environment-resistance of our novel silica AR coating is ten times higher than that of traditional ones. The promotions of the coating performances benefit from its micropore structure(～0.4 nm) with which water molecule can be effectively prevented. With its high transmittance，good mechanical properties and high environment-resistance，this kind of novel coating has a potential application in the field of solar glass modification to improve its anti-reflective properties.
[1] Lee C S，Kim E K，Kim J Y，et al. Metals and Materials International，2012，18(5)：869. [2] Prakash S S，Brinker C J，Hurd A J. Nature，1995，374：439. [3] Asefa T，MacLachlan M J，Coombs N，et al. Nature，1999，402：867. [4] Li Ying，Zhao Gaoyang，Ren Yang，et al. Surf. Interface Anal., 2011，43：1199. [5] Hsu Chenghsing，He Yida，Yang Shufong. Cryst. Res. Technol.，2011，46(1)：65. [6] Solaga C T. Applied Optics，1981，20(20)：3464. [7] Nostell P，Roos A，Karlsson B. Thin Solid Films，1999，351(1-2)：170. [8] Wang X D，Shen J J. Sol-Gel Sci. Technol.，2010，53：322. [9] Rrene P，Priotton J J，Beaurain L，et al. Sol-Gel Sci. Technol.，2000，19：533. [10] Thomas I M. Applied Optics，1992，31(28)：6145. [11] Wu G M，Wang J，Shen J J，et al. Non-Cryst. Solids，2000，275：169. [12] Zhang Y L，Zhang X X，Ye H P，et al. Materials Letters，2012，69：86. [13] YAO Lan-fang，LU Feng-qin，YUE Chun-xiao，et al(姚兰芳，鲁凤芹，岳春晓，等). J. Chin. Ceram. Soc.(硅酸盐学报)，2008，36(2)：139. [14] YANG Yu-jie，ZHANG Lei，XU Yao, et al(杨瑜杰，张 磊，徐 耀，等). High Power Laser and Particle Beams(强激光与粒子束)，2008，20(9)：935. [15] Chi F T，Yan L H，Lv H B. Materials Letters，2011，65：1095. [16] Vicente G S，Bayon R，German N，et al. Thin Solid Films，2009，517(10)：3157. [17] Wongcharee K，Brungs M，Chaplin R. J，et al. Sol-Gel Sci. Technol.，2002，25：215. [18] YAN Liang-hong，CHI Fang-ting，JIANG Xiao-dong，et al(晏良宏，匙芳廷，蒋晓东，等). J. Inorg. Mater.(无机材料学报)，2007，22(6)：1247. [19] CHU Jun-hao, MA Jian-hua, MENG Xiang-jian，et al(褚君浩，马建华，孟祥建，等). CN Patent 1544324A，2004. [20] Xi J Q，Schubert M F，Kim J K，et al. Nature Photonics，2007，1：176. [21] Mehner A，Dong J，Prenzel T J, et al. Sol-Gel Sci. Technol.，2010，54: 355. [22] Wang Z Y，Stein A. Mater. Chem.，2008，20：1029.
