热处理温度对蛋白石晶体的影响

 采用等体积快速混合法制备了不同粒径的单分散SiO₂微球,通过重力垂直沉降自组装形成了蛋白石模板,研究了热处理温度对蛋白石晶体模板形貌、结构与光学性能的影响。SEM,TG-DSC,UV-Vis等分析表明：热处理可提高组装微球的粘合性与模板的机械强度;SiO₂胶体模板煅烧温度在700～800 ℃较为合适;热处理能够改变蛋白石晶体光子带隙的位置,随着煅烧温度的升高,带隙发生蓝移并且带隙逐渐变窄。     

圆柱形蛋白石和反蛋白石结构光子晶体的制备及其光学性质

研究了在圆柱曲面基底上自组装空心和实心的圆柱形蛋白石和反蛋白石结构光子晶体的方法. 用垂直沉积法在不同曲率半径的毛细管内自组装了空心圆柱形聚苯乙烯(PS)蛋白石结构光子晶体薄膜和二氧化硅 (SiO₂) 反蛋白石结构薄膜; 用类重力沉积法制得实心圆柱形蛋白石和反蛋白石结构光子晶体, 并讨论了这一生长方式中的状态变化过程及影响因素. 用扫描电子显微镜对样品内部结构进行了表征, 用光谱仪测试了光子晶体薄膜的反射光谱, 结果表明: 基底曲率半径和微球粒径的大小是影响空心蛋白石和反蛋白石薄膜质量的主要因素; 微球大小是影响实心结构有序性的主要因素. 关键词： 反蛋白石 空心圆柱 溶胶凝胶协同自组装     

孔径梯度变化的聚苯乙烯多孔薄膜的制备

 为了对聚合物多孔材料的微观孔结构进行控制,利用垂直沉积技术,制备了蛋白石结构和多层异质结构的SiO₂胶体晶体,并通过模板导向前驱物填充手段,获得了反蛋白石结构和孔径梯度变化的聚苯乙烯多孔薄膜。扫描电镜分析表明,聚苯乙烯多孔结构精确复制了原始模板的反结构。光学透射谱显示,填充聚苯乙烯后复合蛋白石光子禁带位置相对原始模板发生红移,除去模板后,光子禁带位置发生蓝移。根据布拉格衍射方程,计算出胶体晶体模板空隙的填充分数。     

ZrO2/SiO2溶胶-凝胶薄膜膜层间的渗透行为

 分别以丙醇锆和正硅酸乙酯为原料，采用溶胶-凝胶工艺制备了性能稳定的ZrO₂和SiO₂溶胶。用旋转镀膜法在K9玻璃上分别制备了单层SiO₂薄膜、单层ZrO₂薄膜、ZrO₂/ SiO₂双层膜和SiO₂/ZrO₂双层膜。采用原子力显微镜观察了薄膜的表面形貌，用椭偏仪测量薄膜的厚度与折射率，用紫外-可见光分光光度计测量了薄膜的透射率。对薄膜的透射光谱和椭偏仪模拟的数据进行分析，发现SiO₂/ZrO₂双层膜之间的渗透十分明显，而ZrO₂/SiO₂双层膜之间几乎不发生渗透。利用TFCalc模系设计软件,采用三层膜模型对薄膜的透射率进行模拟，得出的透射曲线与用紫外-可见光分光光度计测量的透射曲线十分符合。     

采用溶胶凝胶协同自组装与光刻相结合的方法在反蛋白石结构薄膜中引入二维缺陷

采用溶胶凝胶协同自组装与光刻相结合的方法,在光子晶体反蛋白石结构中引入缺陷,通过溶胶凝胶协同自组装方法在硅片上垂直沉积胶体晶体复合薄膜,把BP212正性光刻胶均匀旋涂在复合薄膜上,通过曝光、显影等光刻工艺,把掩膜版图案复制在复合薄膜上,用此样品再次垂直沉积一层复合薄膜,使图案被复合薄膜覆盖.最后去除胶体微球与光刻胶图案,从而在反蛋白石结构中引入缺陷,用扫描电子显微镜对样品进行表征.分析了光刻胶图案对胶体微球排列的影响.     

用SCLC法研究低k多孔SiO2:F薄膜的隙态密度

用溶胶-凝胶法制备了低k多孔SiO₂:F薄膜，用空间电荷限制电流法(SCLC)研究了多孔SiO₂:F薄膜中的隙态密度以及掺F量对隙态密度的影响，得到了平衡费米能级附近的隙态密度约为7×10¹⁵cm^-3·eV^-1，以及带隙中隙态随能量的分布. 并对造成隙态的主要原因也进行了讨论.     

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。     

沉降介质对单分散SiO2微球重力组装欧泊模板的影响

 以氨水作催化剂、正硅酸乙酯为硅源、乙醇为溶剂,采用改进溶胶-凝胶法制备了系列单分散SiO₂微球,研究了平均粒径为250,280,320 nm单分散SiO₂微球在水、无水乙醇、丙酮等介质中的沉降与自组装过程。还对单分散体系重力沉降组装欧泊模板的形成机理进行了讨论。SEM表明,微球在无水乙醇和丙酮沉降介质中均能组装形成3维有序密堆积结构的欧泊,但在无水乙醇中要优于在丙酮中。沉降速度实验表明,相同粒径的单分散SiO₂微球在水、乙醇、丙酮作为沉降介质中的沉降速度相差并不大,沉降介质对重力水平沉降组装模板的影响主要是由于其表面张力与粘度不同造成的。     

高折射率光学薄膜的化学法制备研究

 报道了一种以ZrOC₁₂·8H₂O为源,溶胶-凝胶法制备高激光负载高折射率薄膜的新方法。薄膜采用旋转镀膜法制备,对薄膜的结构、光学特性及激光损伤阈值进行了测量,有机粘接剂对薄膜折射率及机械强度的影响也作了探讨。以该薄膜与SiO₂溶胶凝胶膜交替涂覆制成的多层高反膜,剩余透过率仅0.98%,激光损伤阈值达16J/cm²（3ns）。     

超低密度SiO2气凝胶的制备及成型研究

 以正硅酸乙酯(TEOS)为硅源，采用酸碱二步催化溶胶-凝胶法，结合超临界干燥技术制备了超低密度SiO₂气凝胶,最低密度为3.4 mg/cm³；进一步结合成型工艺，在解决了模具设计和脱模技术后制备了具有不同密度的柱状和微型套筒样品，密度10～50 mg/cm³。研究了水、催化剂、稀释剂对二步溶胶-凝胶过程的影响，获得了制备低密度SiO₂气凝胶的最佳条件。利用扫描电镜、孔径分布及比表面积测试仪等对SiO₂气凝胶微结构进行了研究。结果表明，获得的超低密度SiO₂气凝胶具有较好的纳米网络，平均孔径18.9 nm，还具有高比表面积898 9 m²/g。     

Fabrication of Colloidal Photonic Crystals with Heterostructure by Spin-Coating Method

Colloidal photonic crystal heterostructures, composed of two opaline photonic crystal films of silica spheres with different diameters, are fabricated by a two-step spin-coating method. Scanning electron microscopy （SEM） and UV-vis spectrophotometer are used to characterize the heterostructures. The SEM images show good ordering of the two-layer colloidal crystals constituting the heterostructures. The transmission spectra measured from the （111） plane in the heterostructure show that the composite colloidal photonic crystals have double photonic stop bands. Furthermore, when the sizes of the silica spheres used for fabricating the composite photonic crystal are slightly different, the transmission spectrum shows that the composite photonic crystals have more extended bandgap than that of the individual photonic crystals due to partial overlapping of its two photonic stop bands.     

中红外完全带隙Si反蛋白石光子晶体的制备与光学性能研究

通过溶剂蒸发对流自组装法制备SiO2胶体晶体,采用低压化学气相沉积法填充Si,制备得到Si反蛋白石(opal)三维光子晶体.采用扫描电子显微镜对Si反opal的显微形貌进行表征,采用平面波展开法理论模拟Si反opal的光子带隙,采用傅里叶变换红外光谱仪测试其光学性能.研究结果表明:Si在SiO2微球空隙内填充致密均匀,显微红外光谱测试的光子带隙反射峰位置及带宽与理论计算基本符合.变角度反射光谱测试表明,Si反opal沿不同角度入射时在中心波长3319nm处均存在明显的反射峰,证明其具有完全光子带隙,带隙位于中红外大气窗口区域.     

Synthesis of PS colloidal crystal templates and ordered ZnO porous thin films by dip-drawing method

Polystyrene spheres (PS) were synthesized by an emulsifier-free emulsion polymerization technique and the PS colloidal crystal templates were assembled orderly on clean glass substrates by dip-drawing method from emulsion of PS. Porous ZnO thin films were prepared by filling the ZnO sol into the spaces among the close-packed PS templates and then annealing to remove the PS templates. The effects of ZnO precursor sol concentration and dipping time in sol on the porous structure of the thin films were studied. The results showed an ordered ZnO porous thin film with designed pore size that depended on the sol concentration and PS size could be obtained. And the shrinkage of pore diameter was about 30-43%. X-ray diffraction (XRD) spectra indicated the thin film was wurtzite structure. The transmittance spectrum showed that optical transmittance decreased with the decrease of wavelength, but kept above 80% optical transmittances beyond the wavelength of 550 nm. Optical band gap of the porous ZnO thin film (fired at 500 °C) was 3.22 eV.     

Enhanced photoluminescence from three-dimensional ZnO photonic crystals

We have fabricated optically active ZnO inverse opals by infiltrating polystyrene (PS) opal templates using an electrodeposition process. Compared with bare ZnO films also prepared by electrodeposition, the three-dimensional (3D) ordered ZnO structure exhibits markedly enhanced photoluminescence. The effect of photonic band gap on PL spectra is also clearly observed from the ZnO inverse opal structure.     

Structural and cathodoluminiscent properties of Zr0.95Ce0.05O2 nanopowders prepared by sol-gel and template methods

Nanopowders of Zr_0.95Ce_0.05O₂ composition have been prepared by a standard Pechini-type sol-gel process and by means of a colloidal crystal template approach. In the latter method, inverse opal Zr_0.95Ce_0.05O₂ powders were fabricated employing poly(methyl methacrylate) (PMMA) colloidal crystals as a template. The effects of the two different synthesis routes on the structure and microstructural characteristics of the prepared nanopowders were evaluated by X-ray diffraction and scanning electron microscopy. For both preparation routes, the X-ray diffraction analysis has shown that a tetragonal fluorite structure is formed with a crystallite size of ∼35-40 nm. The scanning electron microscopy measurements indicate that the powder obtained by the sol-gel Pechini-type process is comprised of nanoparticles that are arranged in agglomerates with shape and size relatively uniform whereas the inverse opal Zr_0.95Ce_0.05O₂ nanopowders exhibit the formation of macropores with a mean size of ∼100 nm. The cathodoluminescence spectra of the prepared Zr_0.95Ce_0.05O₂ nanomaterials have been measured in the 300-800 nm wavelength range. The powder prepared by sol-gel method yields a broad emission band centered at 482 nm whereas the emission from the inverse opal preparation is considerably less intense.     

Mid infrared band gap properties of 3-dimensional silicon inverse opal photonic crystal

By the solvent vaporization convection self-assembly method, 1.86 μm silica microspheres were assembled into a colloidal crystal template with long-range order. High refractive index silicon was then filled in the voids of the silica template by the low pressure chemical vapor deposition method. A 3-dimensional silicon inverse opal photonic crystal was obtained with a photonic band gap simulated by a plane wave expansion method. Its micro modality and photonic band gap properties were characterized by scanning electron microscopy and Fourier transform IR spectrometer. There was a good agreement between the measured spectra and the simulated results. The tilt-angle reflectance spectra showed that an obvious reflection peak at 3319 nm stayed in existence with different incidence directions. This result proved that silicon inverse opal has a complete photonic band gap in the mid infrared range. This study opens up an opportunity to create Si-based photonic crystal devices for atmosphere mid infrared photodetection.     

Highly-Ordered Ferroelectric Photonic Crystals

Highly-ordered, ferroelectric, Pb-doped Ba0.7Sr0.3TiO3, inverse opal thin films were fabricated using a sol-gel spin coating technique. The excellent crystal quality is evident from the SEM images and the good agreement between the theory and experiments.     

Development of highly-ordered, ferroelectric inverse opal films using sol–gel infiltration

Highly-ordered, ferroelectric, Pb-doped Ba_0.7Sr_0.3TiO₃, inverse opal films were fabricated by spin-coating a sol–gel precursor into a polystyrene artificial opal template followed by heat treatment. Thin films of the ferroelectric were independently studied and were shown to exhibit good dielectric properties and high refractive indices. The excellent quality of the final inverse opal film using this spin-coating infiltration method was confirmed by scanning electron microscopy images and the good correspondence between optical reflection data and theoretical simulations. Using this method, the structural and material parameters of the final ferroelectric inverse opal film were easily adjusted by template heating and through repeated infiltrations, without changes in the initial template or precursor. Also, crack-free inverse opal thin films were fabricated over areas comparable to that of the initial crack-free polystyrene template (100 by 100 m²). PACS  78.67.n; 81.20.Fw; 77.84.Dy