Spin coating process of sol-gel silicate films deposition: Effect of spin speed and processing temperature

The effect of two factors having the most important influence on spin coating process of sol-gel films: the spin speed and the temperature (of the substrate and the applied solution) during film deposition is discussed. It is shown, that film thickness and thickness uniformity are determined by centrifugal driving force dynamics, viscous polymer rheology, solvent evaporation dynamics, and film porous microstructure.     

Effect of processing temperature during spin-on application on the properties of sol-gel silica films

The effect of the temperature (of the substrate and the solution) during film deposition on spin coating process of sol-gel films is discussed. The increase of substrate temperature as well as coating solution liquid temperature leads to formation of thicker films with higher porosity. The temperature dependence of films thickness is mainly determined by the change of solvent vapour pressure with consideration for the change of liquid viscosity.     

Modification of micro-cantilever sensors with sol-gels to enhance performance and immobilize chemically selective phases

A chemical sensor based on the deflection of a surface modified silicon micro-cantilever is presented. A thin film of sol-gel was applied to one side of the micro-cantilever surface using a spin coating procedure. The sensor has been shown to give different responses to vapor phase analytes of varying chemical composition, as well as to varying concentrations of a given analyte. Ethanol, a highly polar molecule, exhibits a strong affinity for the polar sol-gel coating resulting in a large response; pentane, a non-polar hydrocarbon, shows very little response. The sol-gel coating has also been shown to function as a backbone for the immobilization of chemically selective phases on the cantilever surface. Reaction of the sol-gel film with chlorotriethoxysilane and subsequent capping of the remaining reactive surface silanols with hexamethyldisilizane increases the non-polar nature of the film. This results in an increase in the response of the sensor to non-polar analytes. The effects of film thickness and cantilever structure thickness on response were also investigated.     

Development of Anti-Reflection (AR) Coating on Plastic Panels for Display Applications

Traditionally, various vacuum-based processes have been used for producing interference-type anti-reflection (AR) coatings on large area substrates for different commercial applications. In this paper, the development of sol-gel derived AR coating on large plastic substrates for display application is presented. The sol-gel dip coating process was used to deposit thin films on large size plastic panels. By developing sols with different refractive indices, multi-layer thin-film AR coating stacks were designed and fabricated. These coatings possess good uniformity and meet stringent automotive specifications. This technology has been commercialized successfully for dashboard instrument panel application in Toyota's new hybrid engine car, named Prius.In this paper, AR coatings prepared by the sol-gel process are reviewed. The basic design concept for an AR coating, the coating preparation procedure, and important parameters of the solution coating process are discussed. Optical constants of the coating materials were characterized by using spectroscopic ellipsometry. Optical, mechanical and environmental tests were performed on the sol-gel derived AR coating stack. The sol-gel derived AR coating possesses equivalent or superior properties when compared to the major commercially available AR coating products.     

Fibre optic chemical sensors based on evanescent wave interactions in sol-gel-derived porous coatings

A simple, low-cost technique for fabricating reagent-mediated fibre-optic chemical sensors (optrodes) is described and the performance of a range of such sensors is reported. The technique is based on coating an unclad portion of an optical fibre with a microporous glass film prepared by the sol-gel process. Although tip- and side-coating are both possible with this technique, the latter, which employs evanescent wave interactions, offers particular advantages in terms of sensor performance, control of sensitivity and quality of coating. The sol-gel-derived film is used to provide a robust support matrix in which analyte-sensitive dyes are entrapped and into which smaller analyte molecules may diffuse. The benefits of this sol-gel approach to sensor fabrication are illustrated by results from a range of sensors for pH, ammonia and oxygen based on both evanescent wave absorption and evanescent wave excitation of fluorescence.     

不同厚度三倍频SiO2增透膜的设计、制备与改性

本文通过光学计算设计了具有不同厚度的三倍频增透膜。以氨水为催化剂、正硅酸乙酯(TEOS)为前驱体,通过溶胶-凝胶(Sol-Gel)技术制得SiO2溶胶;采用浸渍提拉法镀膜得到符合设计要求的三倍频增透膜。研究结果表明,增透膜的耐磨擦性能随着膜层厚度的增大而增大,本文制得的厚度达到200 nm以上的三倍频增透膜耐磨擦性能显著优于传统的1/4波长三倍频增透膜。此外,本文以甲基含氢硅油为膜表面修饰剂,提出一种全新的超快的表面疏水性改性的方法。经该方法处理后,增透膜由亲水膜转变为疏水膜,对水的接触角从23.4°增大至95°,增透膜的耐环境性显著提高。     

Thin films of functionalized amorphous silica for immunosensors application

Within the framework of the development of an optical immunosensor, the sol-gel process has been used to prepare a thin film of amorphous silica, deposited by spin coating on a gold-coated glass slide, and possessing chemically active functional groups (SH, NH₂...). After activation of the sol-gel film in aqueous buffers by a bifunctional coupling agent, biological molecules such as antibodies could be covalently bonded on or inside the sol-gel film. Therefore, the behavior in aqueous solutions of the functionalized silica thin films has been analysed by Surface Plasmon Resonance (SPR) and guided wave propagation. Results show a modification of the thickness and of the refractive index of the silica film. Pore size range has been deduced by the infiltration of different molecular weight dextran molecules diluted in water into the sol-gel material. Immunosassays have demonstrated biological activity of antibodies which are covalently linked to or entraped in the sol-gel film.     

Macroporous Silicate Films by Dip-Coating

Macroporous silicate thick films were prepared by the sol-gel dip-coating method accompanied by the phase separation using the composition of methyl-trimethoxysilane (MTMS), nitric acid and dimethylformamide (DMF). The morphology of the film varied to a large extent depending on the time difference between hydrolysis and dipping of the coating solution. The films prepared by early coating had inhomogeneous submicrometer-sized pores on the surface of the film. At increased reaction times, relatively narrow sized internal macropores were observed and their size gradually decreased with the increase of reaction time.     

Thickness, Morphology and Structure of Sol-Gel Hybrid Films: I—The Role of the Precursor Solution's Ageing

The physical properties of inorganic-organic sol-gel hybrid films are determined by a large number of processing parameters, as the initial recipe, the catalysis conditions and the film deposition technique. This work focuses on the influence of the precursor solution's ageing on the quality and structure of hybrid silica-polytetrahydrofuran films, prepared by spin coating. The inorganic precursor, tetraethylorthosilicate, was hydrolysed under acid catalysis and using ethanol as co-solvent. The hydrolysis molar ratio (R) was fixed at 4. Different polymer concentrations of two average molecular weights (M _n = 650 and 2900) were added to the initial colloidal solutions. Ageing took place in open containers. The thickness and surface texture parameters of the films were determined by profilometry, and their structures studied by FTIR. It is shown that the films' thickness increases with the ageing of the precursor solution, more steeply for the hybrid films with higher polymer content and higher M _n. The best films obtained, which present the highest thickness and the lowest relative roughness, are those prepared from the most aged solutions. The FTIR results show that the films' porosity increases with the ageing of the precursor solution, and that the distribution of oligomeric species in solution is maintained upon film deposition. Therefore, the structure of the film is essentially determined by the extension of the condensation reactions until the spinning moment.     

CoO—CuO—SiO2三元系统着色涂层的研究

利用溶胶-凝胶法制备反射膜、抗反射膜以及着色涂层的研究近年来较引人注目。山本雄二等报道过CoO-SiO_2、CuO-SiO_2、NiO-SiO_2等二元系统着色涂层,涂层的颜色基本上与其中所包含的有色离子颜色相同。本文采用溶胶-凝胶法制备了CoO-CuO-SiO_2着色涂层,得到了具有Co~(2+)和Cu~(2+)的混合颜色的着色涂层,并确定了该体系的成膜区。     

超动态法快速制备毛细管色谱柱的研究

用超动态法快速制出了几种非极性毛细管柱,柱效、涂渍效率分别为3000～4500理论塔板/m和65～85%。研究了超动态法中涂渍压力、涂渍液浓度与容量因子的关系;考察了制柱重复性和液膜厚度均匀性;给出了涂渍一般口径和试涂大口径厚液膜毛细管柱的部分结果。     

Effect of film thickness controlled by ink‐jet printing method on the optical properties of an electroluminescent polymer

Ink‐jet printing (IJP) represents a highly promising liquid processed polymer deposition method for the film preparation of functional polymers in photo‐electronic devices. In this report, the results on the IJP of a fluorene‐based electroluminescent polymer, poly(9,9‐dihexylfluorene‐alt‐2,5‐dioctyloxybenzene) (PF6OC8), from a piezoelectric droplet generator are presented. The polymer film thickness has been found to show an approximate linear relation with the number of droplets per unit area; it is thus convenient to control the film thickness by the space of printed dots in IJP process. In comparison, spin coating approach is also used to prepare polymer films with different thicknesses by varying solution concentration and spinning speed. However, it is found that spin coating is difficult to control the film thickness quantitatively. The influence of film thickness on the photoluminescence (PL) properties of PF6OC8 films prepared by IJP and spin coating is comparatively investigated. For both ink‐jet printed and spin coated films, the intensity of PL spectra first increases and then decreases with increase in the film thickness, probably due to the exciton quenching in thicker films. When the polymer film thickness is at nanoscale, the major peak in the PL spectrum is the 0–0 vibronic emission at about 420 nm, and with increase in the film thickness, the 0–1 vibronic peak at about 440 nm becomes dominant. The red‐shifted PL spectra with increase in film thickness show the change from the 2D exciton state to the 3D one. Copyright © 2009 John Wiley & Sons, Ltd.     

Fe_2O_3掺杂TiO_2薄膜对甲基紫溶液光催化降解

甲基紫是一种相当稳定的有机物 ,能被 Ti O2 光催化降解 .本文采用 sol-gel工艺在玻璃表面制得了均匀透明的 Ti O2 薄膜 ,研究了热处理温度、涂覆层数、掺杂 Fe2 O3 等制备工艺 ,以及溶液 p H值和助催化剂H2 O2 等因素对 Ti O2 薄膜的光催化性能和稳定性的影响 .结果表明 ,掺 Fe2 O3 的 Ti O2 薄膜对甲基紫的降解率明显优于未掺 Fe2 O3 的 Ti O2 薄膜 .     

Study on the coating of nano-scale SiO<Subscript>2</Subscript> film on the surface of nanocrystalline Mg-Al layered double hydroxides

Since the layered double hydroxides (abbreviatedas LDHs) were firstly reported to be used as precur-sors of new catalytic materials by S. Miyata[1] in 1971,their preparations, ion-exchanges with the balancinginterlayer anions, structure characteristics an…     

Dielectric properties of Al–Si composite oxide films formed on electropolished and DC-etched aluminum by electrophoretic sol-gel coating and anodizing

Highly pure aluminum specimens (99.99%) after electropolishing and DC-etching were covered with SiO₂ films by electrophoretic sol-gel coating and were anodized in neutral boric acid/borate solutions. Time-variations in cell voltage during electrophoretic sol-gel coating and in anode potential during anodizing were monitored. Structure and dielectric properties of the anodic oxide films were examined by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX), and electrochemical impedance spectroscopy (EIS). It was found that electrophoretic sol-gel coating forms uniform SiO₂ films on the surface of both electropolished and DC-etched specimens. Anodizing of specimens after electrophoretic coating lead to the formation of anodic oxide films consisting of two layers: an inner alumina layer and an outer Al–Si composite oxide layer. The anodic oxide films formed, thus, had slightly higher capacitances than those formed on aluminum without any coating. Higher heating temperatures after electrophoretic deposition caused the increase in capacitance of anodic oxide films more effectively. Anodizing in a boric acid solution after SiO₂ coating on DC-etched foil allowed the anode potential to reach a value higher than 1,000 V, resulting in 39% higher capacitances than those on specimens without SiO₂ film. Dedicated to Professor Su-Il Pyun on the occasion of his 65th birthday.     

Parameters affecting the quality of glass capillary columns prepared by the mercury plug dynamic coating method

Summary The paper presents examinations concerning the ways obtaining glass capillary columns. The mercury plug dynamic coating method used for coating capillary columns was investigated in order to establish haw the efficiency of the columns prepared can be related to the physical properties of stationary phase and the velocity of the coating solution through the capillary tube. It was found that there is an optimum range of the viscosity and velocity of the coating solution within which the highest column efficiency can be obtained. Moreover, the mechanism of the mercury plug dynamic coating method in which the thickness of the obtained film depends on interfacial tension between the mercury and the coating solution was confirmed.     

Room-Temperature Mirror Preparation Using Sol-Gel Chemistry and Laminar-Flow Coating Technique

The CEA/DAM megajoule-class pulsed Nd:glass laser devoted to Inertial Confinement Fusion (ICF) research will require 240 cavity-end mirrors. The approved laser design necessitates 42-cm × 46-cm × 9-cm highly-reflective (HR)-coated substrates representing more than 50 m² of coated area. Prototypes of these dielectric mirrors were prepared with interference quaterwave stacks of SiO₂ and ZrO₂-PVP (PolyVinylPyrrolidone) thin films starting from sol-gel colloidal suspensions (sols). Low refractive index material was based on nanosized silica particles and high refractive index coating solution was made of a composite system. The colloidal/polymeric ratio in the composite system has been optimized regarding refractive index value, laser damage threshold and chemical interactions have been studied using FT-IR spectroscopy. A deposition technique so-called Laminar Flow Coating (LFC) has been associated to sol-gel chemistry for HR laser damage-resistant sol-gel coating development. This novel coating method confirmed its main advantages compared to dipping or spinning processes: coating large flat square substrates at room temperature with small solution consumption, good thickness uniformity, weak edge-effects, induced stress-free coating, good optical properties and laser damage resistance fulfilling.     

Formation and Depth Profiling Analysis of Multilayers Derived from Sol-Gel Processing Using Dynamic SIMS, RBS, and TEM

Silica sol-gel single layer AR coatings are used in high peak power pulsed lasers due to their high laser induced damage threshold (LIDT) and their low refractive index (1.22). We have used sol-gel processing to spin and dip coat multilayers of alternating high index (zirconia/hafnia) and low index (base catalysed silica) sol-gels on to fused silica substrates. When tailored at the correct thickness these stacks have shown >95% reflectivity at 355 nm and normal incidence whilst retaining a high LIDT. Depth profiling using Dynamic Secondary Ion Mass Spectrometry (DSIMS) and Rutherford back scattering (RBS) through these multilayer coatings has revealed the effect of increasing the number of layers in the stack. Results are presented for both spin and dip coated multilayers and a significant difference in the interfacial boundary is seen between the two coating processes. These differences are related to changes in the LIDT of the coatings. Individual layer thicknesses were estimated using this technique and compared to values gained from UV-Visible spectroscopy. TEM analysis of an ion-milled cross-section of the multilayers was performed showing the colloidal silica coatings and the depth of interpenetration of the interfaces.     

Protective Properties of a Sol-Gel Coating on Zinc Coated Steel

Galvanised and galvannealed steels are widely used due to their good corrosion resistance in aqueous solutions. However, when additional protection is required, organic coatings, corrosion inhibitors or conversion coatings are used to improve their corrosion protection. In this work, sol-gel coating was used to improve the corrosion behaviour of these two materials. This paper analyses the final protective properties of a sol-gel coating prepared by basic catalysis and its dependence on the sintering temperature and time of treatment. The influence of the sintering conditions on the galvanised and galvannealed substrates is a decisive factor for the coating quality and for the barrier affect against the aggressive media. While heat treatment time is the controlling factor for the galvannealed steels, the temperature is determining in the case of the galvanised. Corrosion mechanisms for sol-gel galvanised steels did not changed with respect to the uncoated steel. However for galvannealed steel, after coating the mechanism is not purely cathodic.