化学涂膜研究平台进展

研究了甲基硅酮防潮膜溶胶的配制及陈化条件、涂膜方式和膜层后处理条件；研究了二氧化硅增透膜溶胶的配制、陈化及回流条件、涂膜方式和膜层后处理条件；研究了双层膜的制备过程。基本确立了防潮膜溶胶和增透膜溶胶的制备条件，涂膜溶胶的溶剂配比、浓度、过滤及涂膜方式和膜层的后处理工艺，在K9玻璃和熔石英基片上分别完成了防潮膜、增透膜及双层膜的涂膜全过程。并对溶胶及膜层的各项性能进行了测试。     

低温制备防潮耐真空污染二氧化硅减反膜

采用溶胶-凝胶法,以正硅酸乙酯为前驱体,氨水为催化剂,通过六甲基二硅氮烷(HMDS)对溶胶改性,使用提拉法镀膜,并经过低温热处理制备了具有良好防潮抗真空性能的SiO_2减反膜.对薄膜的防潮性能、水接触角、真空抗污染能力、结构等进行了测试表征.结果表明:掺HMDS的溶胶制备的二氧化硅膜层峰值透过率为99.7%;水接触角可达154°;在相对湿度大于90%的环境中保存7天和在二甲基硅油作为污染源的真空环境中放置30天,透过率仅分别下降0.05%和0.35%,防潮耐真空稳定性较未改性薄膜都得到极大提高.     

等离子体结合六甲基二硅胺烷处理提升增透膜抗真空污染性能研究

本文采用溶胶-凝胶法制备了SiO₂增透膜,然后对其进行等离子体结合六甲基二硅胺烷（HMDS）表面改性处理。研究了后处理改性对增透膜表面形貌、微观结构、光学性能及激光损伤性能的影响规律,获得了抗真空有机污染的二氧化硅增透膜。结果表明,增透膜在采用等离子体结合HMDS表面改性处理后,膜层收缩、粗糙度下降、极性羟基等有机基团含量减少;两步后处理改善了增透膜膜层结构和光学性能,显著提高了膜层疏水能力和真空条件下的抗污染性能,并且对溶胶-凝胶二氧化硅增透膜的高损伤阈值属性不产生影响。     

溶胶-凝胶双层三波长增透膜制备

通过理论模拟与实验相结合,研究了以双层膜的方式实现三波长增透的途径。以正硅酸乙酯为前驱体,采用酸催化与碱催化溶胶混合的方式调控了溶胶折射率,并配制了双层复合膜所用的两种溶胶,制备出了351nm处透过率大于99.5%,527nm透过率大于98%,1053nm透过率大于98%的三波长增透膜。用扫描电镜、原子力显微镜观测了膜层结构,用椭偏仪和分光光度计对膜层性能进行了表征。三波长增透膜对高功率激光装置的运行性能提升起到了积极的促进作用。     

溶胶—凝胶工艺提拉法制备二氧化硅增透膜

采用溶胶-凝胶工艺用提拉法在石英基片上制备了具有优良的光学特性、高激光损伤阈值和均匀性良好的多孔二氧化硅单层增透膜和“有机硅-SiO₂”双层增透膜系.考察了提拉速率对透射特性的影响,并比较了提拉法和液面下降法对所制备膜层的厚度的影响.透射光谱测量表明,在钕玻璃高功率激光的基频(1060nm)、倍频和三倍频等重要激光波长处均得到较为理想的增透,透射率达到99%以上.     

掺氟SiO_2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。     

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-凝胶法制备有机硅掺杂有机/无机复合疏水性减反射膜的研究

以正硅酸乙酯(TEOS)和硅油为前驱体,在碱性催化体系中制备出有机硅改性二氧化硅溶胶,采用提拉法获得了具备疏水性能的二氧化硅减反膜。通过透射电镜、扫描探针显微镜、红外光谱、分光光度计、表面轮廓仪等多种方法研究了改性后的膜层性能。在高湿度环境中存放两周后,在波长确定的情况下,常规二氧化硅减反膜透过率由99.2%降到了96.5%,疏水改性膜层透过率仍然高于99%。与常规减反膜相比,疏水改性减反膜在高湿度条件下防止潮气侵蚀的性能得到了大幅度的提高。     

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。     

常压百级洁净度环境中SiO2薄膜稳定性

在常压百级洁净度环境下,采用三种不同折射率的SiO₂溶胶在熔石英基底上涂制四种不同薄膜,利用光学理论计算模拟了三种胶体涂制的膜层稳定性,通过实验考查了膜层光学指标随时间的变化规律。SiO₂薄膜能够显著提升光学元件透射率,但由于膜层表面的大量羟基及其多孔结构,SiO₂薄膜易吸附周围环境中的有机污染物及水分填充膜层孔隙,从而导致膜层折射率发生变化,影响膜层透射率、反射率等光学性能。实验结果发现,三种溶胶凝胶化学膜在常压百级环境中的有效期为80 d(绝对变化率小于0.1%),且三种胶体涂制的膜层稳定性由高到低依次为折射率1.19, 1.15, 1.25的膜层。     

Surface modification on a glass surface with a combination technique of sol-gel and air brushing processes

This study fabricated the large area and optically transparent superhydrophobic silica based films on glass surface with optimized hardness. A silane coupling agent, tetraethoxysilane (TEOS), effectively bonds silica particles onto the glass substrate. Desired surface roughness was obtained by adjusting nano silica particles concentration of the precursors prepared by the sol-gel process. Silica suspension was coated onto the glass substrate by the air brushing methods. This method can deposit a uniform, transparent coating on the glass substrate efficiently. Diluting the precursor by adding ethanol or a mixture of D.I. water and ethanol further improved the transmittance and superhydrophobicity efficiency. The results showed that as the silica particle concentration and the thickness of the coating were increased, the surface roughness was enhanced. Rougher surface displayed a higher superhydrophobicity and lower transmittance. Therefore, the concentration of silica particle, volume of coatings, and the ratio of ethanol and D.I. water are of great importance to deposit a transparent, superhydrophobic coating on glass.     

SiO_2光学增透膜的制备及光学性能

在碱催化体系中以正硅酸乙酯 (TEOS)为前驱体制得SiO2 溶胶 ,采用旋转镀膜法 (spin coating)制备SiO2 光学增透膜。研究了在不同制备条件下对膜层光学性质的影响 ,推算了膜层的折射率及厚度 ,并由此给出膜层孔隙率以及膜层的厚度与转速的关系     

Plasmon based antireflection coatings containing nanostructured Ag and silica medium

The transmittance and scattering of the antireflection (AR) coatings based on nanostructured Ag and silica medium were enhanced by the exploitation of the localized surface plasmon resonance (LSPR). The transmittance and scattering values of AR coatings are relative to the annealing temperature, Ag concentration and thickness of AR coatings. The transmittance values of 95.7% and 97.2% of AR coatings with 0.10 wt.% Ag and annealed at 400 °C were obtained in the visible wavelength for a single-side and double-side coated glass slides, respectively. The enhanced transmittance and scattering of the AR coatings are primarily attributable to the large forward scattering of nanostructured Ag and the lesser refractive indices of Ag/SiO₂ coatings.     

太阳能玻璃表面高强度双层减反膜制备研究

用膜系设计软件设计了λ/4-λ/2的W型的双层减反射薄膜,优化了薄膜的光学常量,并使用溶胶-凝胶技术在玻璃基底上成功镀制了该双层折射率梯度的减反射薄膜.用椭圆偏振光谱仪、紫外-可见-近红外分光光度计、原子力显微镜等分析表征了薄膜的性能.结果表明,镀制了该双层薄膜的玻璃在400 nm～800 nm波段平均透过率增加了近6%,同时薄膜显示出了极佳的机械强度.     

水含量对溶胶-凝胶SiO2增透膜结构和性能的影响

利用正硅酸乙脂(TEOS)的碱催化,溶胶-凝胶法制备多孔SiO₂增透膜.较详细地研究了工艺参量H₂O/TEOS摩尔比对薄膜结构和性能的影响.结果表明,随H₂O/TEOS摩尔比的增大,薄膜厚度、折射率和致密度减小;而薄膜透射率增大.     

太阳能玻璃表面高强度双层减反膜制备研究

用膜系设计软件设计了λ/4-λ/2的W型的双层减反射薄膜,优化了薄膜的光学常量,并使用溶胶-凝胶技术在玻璃基底上成功镀制了该双层折射率梯度的减反射薄膜.用椭圆偏振光谱仪、紫外-可见-近红外分光光度计、原子力显微镜等分析表征了薄膜的性能.结果表明,镀制了该双层薄膜的玻璃在400 nm～800 nm波段平均透过率增加了近6%,同时薄膜显示出了极佳的机械强度.     

Electrical and optical properties of Si-doped indium tin oxides as transparent electrode and anti-reflection coating for solar cells

We have studied the electrical and optical properties of Si-doped indium tin oxides (ITSOs) as transparent electrodes and anti-reflection coatings for Si-based solar cells. The ITSO thin films were obtained by co-sputtering of ITO and SiO₂ targets under target power control. The resistivity of the ITSO thin films deposited at 0.625 in terms of power ratio (ITO/SiO₂) were 391 Ωcm. In this condition, the ITSO thin films showed very high resistivity compared to sputted pure ITO thin films (1.08 × 10⁻³ Ωcm). However, refractive index of ITSO thin films deposited at the same condition at 500 nm is somewhat lowered to 1.97 compared to ITO thin films (2.06). The fabricated graded refractive index AR coatings using ITO, ITSO, and SiO₂ thin films kept over 80% of transmittance regardless of their thickness varing from 97 nm to 1196 nm because of their low extinction coefficient. As the AR coating with graded refractive indices using ITO, ITSO, and SiO₂ layers was applied to general silicon-based solar cell, the current level increased nearly twice more than that of bare silicon solar cell without AR coating.