利用氟硅烷提高溶胶-凝胶SiO2增透膜的疏水性

以正硅酸乙酯为前驱体,氨水为催化剂,采用溶胶 凝胶法制备了二氧化硅增透膜;通过自组装技术,用氟硅烷对膜层进行表面修饰,制得了疏水增透膜,克服了常规增透膜亲水的缺点。采用红外光谱、分光光度计、扫描探针显微镜和静滴接触角测量仪等测试手段分析了薄膜的特性。结果表明：疏水增透膜的峰值透光率为99.7％,疏水角为110°;氟硅烷自组装改性不影响二氧化硅增透膜的光学性能。     

掺氟SiO2增透膜真空环境抗污染能力

以正硅酸乙酯为前驱体,采用氨水为催化剂配制SiO2溶胶,在胶体陈化过程中掺入十二氟庚基丙基三甲氧基硅烷对胶体进行改性,并采用溶胶 凝胶法在K9基片上制备了改性的二氧化硅增透膜,用红外光谱仪、分光光度计、原子力显微镜、椭偏仪、静滴接触角测量仪、N2吸附-脱附对膜层性质进行了分析。结果表明：掺氟的二氧化硅膜层增透膜峰值透光率为99.7%;与水的接触角为129°;与二甲基硅油的接触角达到86°;膜层真空抗污染能力比掺氟前大大提高。     

溶胶-凝胶法制备疏水性自组装SiO2薄膜

 以正硅酸乙酯（TEOS）和六甲基二硅氮烷（HMDS）为前驱体,研究了引入聚乙烯吡咯烷酮（PVP）对膜层的影响,在碱催化条件下制备了改性的二氧化硅溶胶,并采用提拉涂膜的方法在石英基底上涂膜。对不同组分的薄膜,先经热处理或紫外辐照处理,然后用十八烷基三氯硅烷（OTS）/甲苯溶液对膜层表面进行化学修饰,制备出疏水性能良好的纳米二氧化硅自组装薄膜,分析了不同后处理方法对膜层透过率、接触角、膜层表面微观形貌和激光损伤阈值影响。实验结果表明：溶胶中加入PVP提高了膜层的平整度,经OTS改性后膜层疏水性和激光损伤阈值均得到提高。     

溶胶凝胶法制备抗激光损伤SiO2疏水减反射膜

 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。     

水解反应温度对溶胶-凝胶SiO2增透膜光学性能的影响

在制备高激光损伤阈值溶胶-凝胶二氧化硅增透膜的工艺中,水解反应温度对镀膜溶胶的形成和薄膜的光学性能都有很大影响。本文较为详细地研究了这一重要工艺多数对镀膜溶胶的颗粒度、分散性、稳定性的影响,以及它对薄膜增速效果的影响。     

溶胶凝胶法制备抗激光损伤SiO2疏水减反射膜

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。     

溶胶-凝胶法MgF2紫外增透膜的制备和性能研究

采用溶胶-凝胶法,以醋酸镁和氟化氢为原料,以甲醇为溶剂制备了MgF2溶胶,利用浸渍提拉法在洁净石英基片上镀膜,考察了反应温度对溶胶微结构、薄膜结构和性能的影响。样品采用激光动态光散射、透射电镜、X射线粉体衍射仪、紫外-可见光谱仪、原子力显微镜进行表征。结果表明：通过该方法制备的表面平整的低折射率MgF2薄膜,在紫外区具有很好的增透性能,同时在紫外波长355 nm激光的辐照下（脉宽6 ns）,薄膜具有较高的抗激光损伤性能,激光损伤阈值达10.85 J·cm-2。     

杂质对溶胶-凝胶SiO2薄膜激光损伤的影响

采用溶胶-凝胶法制备了含有吸收性杂质和非吸收性杂质的SiO2增透膜,采用波长为1 064 nm的激光对其进行了小光斑激光预处理,对比研究了预处理前后的激光损伤差异,研究表明：激光预处理对于洁净的SiO2薄膜影响不大;含10 μm SiO2颗粒杂质的样品微透镜效应很明显,容易成为损伤起始的种子,激光预处理后情况有所改善;含有CeO2颗粒杂质的样品表现出了很强的吸收性质,损伤阈值降低到不足洁净样品的一半。所有样品激光预处理后损伤形貌未发生变化,透光率峰值均有约50 nm的蓝移。     

溶胶-凝胶SiO2薄膜氨热两步后处理

 以正硅酸乙酯为前驱体,氨水作催化剂,采用溶胶-凝胶法提拉镀制SiO₂双面膜,对薄膜进行氨处理和热处理。采用椭偏仪、分光光度计、红外光谱、扫描探针显微镜、静滴接触角测量仪表征薄膜的特性。研究表明：经氨热两步后处理,膜厚持续减小,折射率经氨处理先增大了0.236,再经热处理又减小了0.202,膜层透光性变好,透过率峰值持续向短波方向移动;经两步后处理的膜面平整度明显变好,与水的接触角先增大到58.92°后减小到38.07°。     

溶胶-凝胶法制备耐磨宽带SiO2/TiO2增透膜

以钛酸正丁酯[Ti(OBu)4]、正硅酸乙酯(TEOS)为原料，采用溶胶—凝胶(sol—gel)提拉方法在K9光学玻璃基片上镀制得高透过的λ／4～λ／2型宽带增透膜。该增透膜的表面均匀性良好，均方根粗糙度(RMS)为1.201，平均粗糙度(RA)为0．934，具有一定的耐擦除性。经200℃热处理，膜层中的OH吸收峰已基本消失，在400～700nm光谱范围的透过率比基片的平均透过率提高6．6％。为实现大面积涂覆“神光”装置主放大器的防爆隔板玻璃，大幅度提高主放大器的抽运效率奠定基础。     

Study on the hydrophobic surfaces prepared by two-step sol-gel process

In this study, the two-step sol-gel process was used to prepare hydrophobic coating films on the glass substrates. The first step was to add hydrogen chloride into TEOS (tetraethoxysilane) solution, and then the second step was to add ammonia into the above reacted solution. We adopted different amount of hydrogen chloride and ammonia to control the sol-gel reaction and observed the change of the viscosity, gelatin period of the solution and contact angles of the coating films. By this method, we created a surface with roughness and then the hydroxyl groups were terminated by adding trimethylchlorosilane (TMCS) to produce a hydrophobic coating layer. The amount of the acid, base and water added in the solution influenced the reaction rate and resulted in the aggregation and condensation of the particles to form rough surfaces. Consequently, the rough surfaces made by aggregation and condensation of the large particles, which were modified by TMCS resulted in higher contact angles (>140°). In this study, a surface with contact angle 150° was obtained.     

Tough ceramic coatings: Carbon nanotube reinforced silica sol-gel

Silica coatings reinforced with carbon nanotubes were produced via sol-gel route using two mixing techniques of the sol-gel precursors, mechanical and ultrasonic mixing, and dip-coating as deposition process on magnesium alloy substrates. Effective incorporation and distribution of 0.1 wt.% of carbon nanotubes in the amorphous silica matrix of the coatings were achieved using both techniques. Fabrication procedure determines the morphological aspects of the coating. Only mechanical mixing process produced coatings dense and free of defects. Nanoindentation technique was used to examine the influence of the fabrication process in the mechanical features of the final coatings, i.e. indentation fracture toughness, Young's modulus and hardness. A maximum toughening effect of about 24% was achieved in silica coatings reinforced with carbon nanotubes produced by the mechanical mixing route. Scanning electron microscopy investigation revealed that the toughening of these reinforced coatings was mainly due to bridging effect of the reinforcement.     

高功率激光宽光谱减反膜的溶胶-凝胶旋转法制备工艺

 采用溶胶-凝胶法用旋转镀膜工艺在K9玻璃基片上制备出了SiO₂和有机硅单层减反膜以及有机硅-SiO₂双层减反膜。考察了旋转速度对SiO₂和有机硅单层膜的中心透射波长、膜层折射率等基本光学性质的影响，实验确定了双层膜的涂敷工艺。透射光谱测量表明，采用本文工艺条件制备的有机硅 SiO₂双层膜在430～800nm范围内透射率达99％以上。     

Transparent water repellent silica films by sol-gel process

Non-wettable surfaces with high contact angles and facile sliding angle of water droplets have received tremendous attention in recent years. The present paper describes the room temperature (∼27 °C) synthesis of dip coated water repellent silica coatings on glass substrates using iso-butyltrimethoxysilane (iso-BTMS) as a co-precursor. Emphasis is given to the influence of the hydrophobic reagent (iso-BTMS) on the water repellent properties of the silica films. Silica sol was prepared by keeping the molar ratio of tetraethoxysilane (TEOS) precursor, methanol (MeOH) solvent, water (H₂O) constant at 1:16.53:8.26 respectively, with 0.01 M NH₄F throughout the experiment and the molar ratio of iso-BTMS/TEOS (M) was varied from 0 to 0.965. The effect of M on the surface structure and hydrophobicity has been researched. The static water contact angle values of the silica films increased from 65° to 140° and water sliding angle values decreased from 42° to 16° with an increase in the M value from 0 to 0.965. The water repellent silica films are thermally stable up to a temperature of 280 °C and above this temperature the film shows hydrophilic behavior. The water repellent silica films were characterized by the Fourier Transform Infrared (FT-IR) Spectroscopy, Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), % of optical transmission, thermal and chemical aging tests, humidity tests, static and dynamic water contact angle measurements.     

改性剂对旋转法SiO2减反膜均匀性的影响

分析了采用旋转涂膜法制备溶胶-凝胶SiO2减反膜过程中条纹缺陷产生的机理,利用含氟醇类试剂对减反膜溶胶进行改性,使溶胶链段柔顺性及流动性得到改善。在光学显微镜下对改性前后的膜层进行了对比和分析,对膜层的表面形貌、表面粗糙度以及透射比等特性进行了表征。结果表明:溶胶改性之后的膜层未出现条纹缺陷,表面粗糙度均方根值从4.55 nm下降到小于1.00 nm,膜层表面质量有了较大提高;改性前后膜层的增透性能相当,在熔石英基片上制备的膜层峰值透射比为99.60%~99.89%,膜层激光损伤阈值为21.0~25.3 J/cm2。     

Sliding behavior of water drops on sol-gel derived hydrophobic silica films

Control on the wettability of solid state materials is a classical and key issue in surface engineering. Optically transparent methyltriethoxysilane (MTES)-based silica films with water sliding angle as low as 9° were successfully prepared by two-step sol-gel co-precursor method. The emphasis is given to the effect of trimethylethoxysilane (TMES) as a co-precursor on water sliding behavior of silica films. The coating sol was prepared with molar ratio of methyltriethoxysilane (MTES), methanol (MeOH), acidic water (0.01 M, oxalic acid) and basic water (12 M, NH₄OH) kept constant at 1:12.73:3.58:3.58 respectively, and the molar ratio of TMES/MTES (M) was varied from 0 to 0.22. The static water contact angle as high as 120° and the water sliding angle as low as 9° was obtained by keeping the molar ratio (M) of TMES/MTES at 0.22. When the modified films were cured at temperature higher than 280 °C, the films became superhydrophilic. Further, the humidity study was carried out at a relative humidity of 90% at 30 °C over 60 days. We characterized the water repellent silica films by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), % of optical transmission, humidity tests and static and dynamic water contact angle (CA) measurements.     

Surface roughness reduction in X-ray mirrors via sol-gel silica coatings

Surface roughness is a key point for all X-ray reflective optics, and is in general obtained through careful polishing and surface finishing. Here we propose a simple and inexpensive procedure to drastically reduce surface roughness: using sol-gel silica coatings. The motivation for this work is the improvement of X-ray mirrors obtained on Si substrate using micro-fabrication technology, where the usual polishing methods cannot be applied. Sol-gel silica layers dramatically reduce surface roughness and enhance the X-ray reflectivity up to acceptable values. The proof-of-principle presented in this paper can be further improved and applied to systems of different nature.     

TMOS based water repellent silica thin films by co-precursor method using TMES as a hydrophobic agent

The present paper describes the room temperature synthesis of dip coated water repellent silica coatings on glass substrates using trimethylethoxysilane (TMES) as a co-precursor. Silica sol was prepared by keeping the molar ratio of tetramethoxysilane (TMOS) precursor, methanol (MeOH) solvent, water (H₂O) constant at 1:29.27:2.09 respectively, with 0.5 M NH₄OH throughout the experiments and the TMES/TMOS molar ratio (M) was varied from 0 to 3.8. It was found that with an increase in M value, the roughness and hydrophobicity of the films increased, however the optical transmission decreased from 93% to 57% in the visible range. The hydrophobic silica films retained their hydrophobicity up to a temperature of 250 °C and above this temperature the films became hydrophilic. The hydrophobic silica thin films were characterized by taking into consideration the surface roughness studies, Fourier transform infrared (FT-IR) spectroscopy, percentage of optical transmission, scanning electron microscopy (SEM) and contact angle measurements.