采用溶胶凝胶法制备得到以正丙醇锆和正硅酸乙酯为前驱体的ZrO₂和SiO₂溶胶，通过TFCalc光学薄膜软件模拟了ZrO₂/SiO₂三层“宽M型”基频二倍频减反膜，并使用提拉法制备得到了该均匀膜层。三层减反膜在527 nm和1053 nm处的透过率约为99.5%，且透过率大于99%的波长范围均超过150 nm。经热处理后的膜层表面均方根粗糙度为1.34 nm，表面平整性良好；并运用1-on-1激光损伤阈值测试方法测得该减反膜的零几率激光损伤阈值达到36.8 J·cm^-2（1064 nm，10.7 ns）。

真空环境中高功率激光装置光学元件表面的有机物污染是限制其负载能力的原因之一。针对装置中常见的有机物污染和三倍频激光溶胶凝胶减反膜，通过精确控制真空环境中污染源的挥发扩散，制备了有机物质量面密度不同的元件表面，定量研究了有机污染物质量面密度对溶胶凝胶减反膜光学性能及损伤特性的影响规律。实验结果表明：样品表面粗糙度、透过率、损伤阈值等的变化量均与有机物质量面密度成正相关。有机污染物沉积量较少时，由于膜层孔隙被填充，膜层的表面粗糙度略有减小；随着沉积量增加，有机物附着影响表面形貌，粗糙度显著增加。溶胶凝胶减反膜在351 nm波长处的光学透过率随着有机物质量面密度的增加而逐渐降低，这与有机物分子改变溶胶凝胶膜孔隙填充比有关。样品表面的激光损伤阈值变化量和损伤面积随着有机物质量面密度的增加而增加，而且不同有机物沉积量的光学表面的损伤形貌存在显著差异。基于实验结果讨论了有机物影响溶胶凝胶减反膜性能的机理，并探讨了高功率激光系统的洁净度控制方法。

以正硅酸乙酯作为前驱体,乙醇作为溶剂,氨水作为催化剂,在碱催化体系下制备了高分散的SiO₂溶胶;然后采用提拉法在不同浓度的SiO₂溶胶涂膜液中制备了四倍频266 nm波长增透的SiO₂减反膜,并对各膜层的性能进行了测试。测试结果表明:在浓度最大的SiO₂溶胶中以4.5 cm·min ^-1的提拉速度制备得到的四倍频SiO₂减反膜的性能最优,其在266 nm处的透过率达到了99.307%,表面粗糙度为1.339 nm,且透过率稳定性优异。

以正硅酸乙酯为原料,采用溶胶-凝胶法制备SiO₂溶胶,通过提拉法涂制多孔SiO₂减反膜,并在多孔SiO₂减反膜上涂制一层甲基三乙氧基硅烷(MTES)预聚体。通过疏水的MTES预聚体涂制在多孔SiO₂减反膜上,对多孔SiO₂减反膜的表面进行改性,以提高膜层的环境稳定性。经过表面改性的复合膜层的透过率峰值可达99.67%,折射率为1.231,水接触角达123.6°,在相对湿度为95%的环境中放置475 d后膜层的峰值透过率为99.09%,稳定性提高明显。膜层表面平整,激光损伤阈值约为24.5 J/cm ²。

以钛酸正丁酯、正硅酸乙酯为前驱体,在薄膜设计软件的辅助下,采用溶胶-凝胶法在K9光学玻璃上制备了λ/4-λ/2-λ/2膜系宽带减反膜。该膜层的光学性能良好,在500~900 nm波长范围内的平均透过率为99.25%,透过率增益随入射角增加而增大,斜入射光入射角从0°增至60°仍能有效覆盖钕玻璃的主吸收峰,此时平均透过率增益从7.2%增至10.2%;在150 ℃下进行热处理后,膜层具有一定的耐擦拭性能,表面均匀性良好,均方根粗糙度为4.00 nm。

The silica suspension was prepared by a sol gel method using tetraethylorthosilicate (TEOS) as precursor and ethanol as solvent. The stability of the sol system was observed by particle size test. The particle size maintained at about 6.5 nm for 4 months. The quartz substrates were coated by a dipping method and heat treated at 200 ℃ and 800 ℃ in a muffle burner. The film transmittance curve moves to short wavelength direction by about 210 nm, and both the transmittance peaks are more than 99.8%. Therefore, the film’ optical properties are excellent. The stabilities of film heat treated at different temperatures were researched in different humidity environments. The transmittances of the films heat treated at 200 ℃ are more than 99.9% and the wavelength of film transmittance peak decreases by about 150 nm. The transmittances of the films heat treated at 800 ℃ reduces by 0.3% and the wavelength of film transmittance peak maintain at 600 nm.

Antireflective coatings prepared by sol gel method are importantly used in high power laser devices, the stability of colloidal, laser induced damage thresholds (LIDTs) and antireflective efficiencies of coatings resulted from different particle sizes silica colloidal suspensions and silica antireflective coatings are studied by controlling different molar ratios of water and tetraethoxysilane (TEOS). The results show that the transmittance of porous silica antireflective films is higher than 99.5% and LIDTs are greater than 62 J/cm2 (1064 nm, 15 ns), the transmittance and LIDTs of smaller particle size silica antireflective film reaches 99.75% and 77.42 J/cm2 (1064 nm, 15 ns), respectively. The average particle sizes of colloidal suspensions increase with the mol ratio of H2OTEOS, the particle size quickly increases when the molar ratio of water and ester is greater than 3.5. The solution with particle size below 10 nm has excellent stability, and the particle size and viscosity of the solution is almost not unchanged. The stability of films with different particle sizes in different humidities is researched, all the films′ transmittance in high humidity drops and the film with larger particle size has more obvious decrease in transmittance, and therefore the chemical films are more suitable for the use in low humidity environment.

溶胶凝胶法制备减反膜在高功率激光装置中有着重要运用，通过控制水与正硅酸乙酯(TEOS)不同特质的量之比制备不同粒径大小的二氧化硅悬胶体及二氧化硅减反膜，可以研究悬胶体粒径大小对溶液及膜层的激光破坏阈值、光学减反效率稳定性影响。结果表明制备获得的多孔性SiO2减反膜透射率均高于99.5%，激光破坏阈值均大于62 J/cm2(1064 nm,15 ns)，其中粒径小的SiO2减反膜透射率达到99.75%，激光破坏阈值高达77.42 J/cm2(1064 nm,15 ns)。随着水酯物质的量比值增大，悬胶体溶液平均粒径增大，当水酯物质的量比值大于3.5时粒径增大幅度加快；粒径在10 nm以下的溶液具有优异的稳定性，溶液颗粒大小、粘度等性能基本保持不变。在不同湿度环境下研究不同粒径膜层的稳定性，所有膜层在高湿度环境中透射率有所下降，其中大粒径膜层下降更明显，化学膜更适合在湿度低的环境下使用。