In‐Situ‐Charakterisierung optischer Mehrschichtsysteme in Großflächen‐ Produktionsanlagen

The paper discusses approaches to the insitu analysis of optical multi‐layer coating stacks such as mirror coatings, AR coatings or lowE layer stacks on large‐area substrates in production environments. The stable production of complex layer systems requires in‐situ analysis systems that are able to provide spectral information and optical performance data, but also yield thickness information for individual layers and thus aide the operating staff in detailed analyzing deviations from the production target stack. Solutions incorporating in‐situ optical reflectance, transmittance and ellipsometry measurements wi^th optical data being collected not only for the completed layer stack, but also at intermediate coating stages, are discussed and the accuracy, robustness and stability of different measurement systems and computation strategies are compared.     

Dünnschichtfilter in der Telekommunikation

Market forces are pushing the performance of optics to their limits. Optical components must be developed to provide the best possible combination of manufacturability, performance and price. One vital step to success in creating WDM optics lies in a discipline that is often overlooked or misunderstood – coating engineering. A key technology for controlling light in WDM systems is the optical filter, which performs functions from simple filtering in multiplexers and demultiplexers, to more sophisticated functions in optical amplifiers, modulators and test equipment. The basic tool of multiplexing and demultiplexing devices, thin film filters offer accurate center wavelength, broad flattop passband and high isolation from adjacent and nonadjacent channels. Thin film filters are widely used for gain flattening, band splitting, C and L band separation and combining amplifier‐pump beams. Choosing the right thin‐film‐deposition process is essential for the efficiency and productivity of vacuum coating systems. LEYBOLD OPTICS has developed and optimized a comprehensive range of vacuum coating processes and process tools. LEYBOLD OPTICS has been proven the ability of producing shift‐free coatings on large substrate areas by means of PIAD (Plasma Ion Assisted Deposition) in many applications over the past ten years. The low loss and stress values achieved, especially with silica and tantala films, allows besides the production of narrow band pass filters (DWDM, CWDM) also the production of gain flattening filters (GFF). PIAD is considerably improving the properties of evaporated thin films by high energy ion bombardment during the growing of the film. PIAD allows to produce dense shift free thin films with high refractive index, good adhesion and extremely low absorption. With the Advanced Plasma Source (APS) LEYBOLD OPTICS has developed a high power plasma source for PIAD. The APS provides high ion current densities over a large surface area in a neutral plasma to produce high quality layers at a high productivity.     

Rotatable Magnetron Sputter Technologyfor Large Area Glass and Web Coating

Over the last few decades, magnetron sputtering has become a major coating technology for depositing high quality thin films. The ease of scalability, while maintaining excellent control of all crucial layer parameters, made it appropriate for large area substrates and high mass productivity. The introduction of the rotating cylindrical magnetron concept in the nineties has further contributed to the success of sputtering in large area coating of rigid and flexible substrates. The rotatable sputtering technology does not only contribute significantly to a reduction in cost‐of‐ownership (higher target material consumption, more system throughput and up‐time …), it opens new perspectives in advanced coating applications where tolerances are narrow and requirements are high. In this paper, we will discuss the advantages of using rotatable target technology in large area coaters, whereby we will focus on the issues related to the sputter deposition on rigid and flexible substrates.     

Single‐Walled Carbon‐Nanotube Networks on Large‐Area Glass Substrate by the Dip‐Coating Method

Highly uniform and large‐area single‐walled carbon‐nanotube (SWNT) networks are realized by the dip‐coating method, which is based on fundamental fluid‐dynamic phenomena such as capillary condensation and surface tension. The changes in the polarity and hydration properties of the substrate affect the morphology of the SWNT networks and result in nonlinear growth of the networks in the repetitive dip‐coating process. The density and the thickness of the SWNT networks are controlled by processing variables including number of dip coatings, concentration of SWNT colloidal solution, and withdrawal velocity. The networks have uniform sheet resistances and high optical transmittance in the visible wavelength range.     

Quantitative SIMS Tiefenprofil Analyse

Quantitative secondary ion mass spectrometry (SIMS) Today, thin surface coatings have become an integral construction element in mechanical engineering, optics, electronics, automotive, etc.. The layer thicknesses range from a few nanometers, e.g. in optical filters or low‐E coating systems, via micrometerrange coatings for friction and wear reduction, to thick galvanic coatings or spray coatings of up to 100 microns thickness or more. Crucial for the development and application of such layers is the availability of analytical methods, which are capable of characterizing e.g. chemical composition of layers with high lateral and depth resolution. Only with knowledge of the internal composition coating systems can be systematically optimized and errors in coating processes can be identified. Quantitative SIMS depth profile analysis is a method that can determine the chemical composition of single or multi‐layer systems with a depth resolution in the nanometer range, making it an indispensable tool in the coating and surface technology. This article explains the technical basics of secondary ion mass spectrometry (SIMS) and shows several practical examples from industry.     

Herstellung HVOF gespritzter,feinststrukturierter Cermetschichten unter Verwendung von feinen WC‐12Co Pulvern

Manufacturing of HVOF sprayed, finest structured cermet coatings using fine WC‐12Co powders The continuous increase in productivity and performance of modern sheet metal forming processes combined with the employment of novel, high strength materials cause high wear on tool systems. Coating technologies like thermal spraying provide a high potential to functionalize and to protect the surface of forming tools. However, it has to be ensured that the high shape and dimensional accuracy of the tool contour is preserved after the application of a wear protective coating. This aim cannot be achieved using currently applied, thermally sprayed coating systems with conventional, coarse grained microstructure. To solve this problem, novel finest structured coatings have been developed in this study by thermal spraying of fine WC‐12Co powders using the HVOF technique. For this purpose the influence of varying HVOF combustion gas compositions on the spray process as well as on the corresponding coating properties has been investigated. Next to a high surface quality the focus was placed on achieving coatings with high hardness and corresponding high wear resistance, low porosity as well as a good adhesive strength on the substrate material.     

The production of porous and chemically reactive coatings by magnetron sputtering

High surface area materials can have a number of applications including use as pyrophoric devices, sensors, laser mirrors, filters, thermal barriers and catalysts. The aim of this work was to deposit highly porous thin films capable of undergoing a spontaneous pyrophoric reaction and igniting a suitable substrate material. Magnetron sputtering was the chosen deposition technique as it enables reproducible deposition of coatings, with closely controlled, almost uniform, thickness and morphologies over extended surfaces.A number of magnetron magnetic configurations were investigated and deposition conditions were varied in order to control the surface area of the films and, thereby, optimise the pyrophoric behaviour. As a consequence, pyrophoric coatings were produced with ignition temperatures dependent on the deposition conditions and substrate material/topography. When deposited on combustible substrates, these coating/substrate systems formed simple pyrotechnic devices in a one-stage process. The main thermal signal emitted by these devices was dependent on the substrate material only.     

On‐line Quality Control of Coated Glass. On‐line Qualitätskontrolle von beschichtetem Glas

Properties of optical coatings (e.g. low‐e or solar control) can be described and controlled using transmittance, reflectance and sheet resistance measurements. Multiple in situ transmittance measurement points allow a quick response to adjust different coating processes (layer thickness and homogeneity). For the final characterization of the coated substrate ex situ transmittance, reflectance and sheet resistance measurements are used. Accurate and reproducible measurements in a combination with Reverse Engineering methods admit monitoring all layers and in this way detecting slight drifts.     

Uniformity of film thickness on rotating planetary planar substrates

For the purposes of obtaining a number of components with nearly identical thickness distributions over the substrate area and of minimizing the inhomogeneities of the film, it is logical to presume that a substrate rotating on its own axis and revolving around another axis will give more uniformity in film thickness than a substrate only revolving around one axis. In relation to the practical applications, an investigation has been undertaken to study the refinement that can be achieved by using a planar planetary substrate holder.It is shown theoretically that the use of the planetary substrate holder under ideal conditions of source and geometry does not offer any further improvement in uniformity of thickness over the conventional rotary work-holder. It is also shown that the geometrical parameters alone have little influence over the uniformity achieved on a planetary substrate, because of the complex cyclidal motion of any point on it. However, for any given geometry, a non-integral speed ratio of the planetary substrate and the work-holder shows considerably less variation in thickness over the substrate area.     

Wavefront control of SiO2-based ultraviolet narrow-bandpass filters prepared by plasma ion-assisted deposition

Metal oxide layers produced by plasma ion-assisted deposition are extensively used for complex optical coatings due to the availability of materials, the high packing density of films, and the smooth surfaces. Stringent optical surface figure specifications necessary for both laser optics and precision optics require film stress to be well-controlled and surface deformation to be corrected or compensated. SiO(2)- based single-cavity UV narrow-bandpass filters were prepared by plasma ion-assisted deposition. The correlation between film stress, refractive index, deposition parameters, and postdeposition annealing was established. The film stress was calculated based on interferometric surface deformation. The refractive index and film thickness were determined by means of variable angle spectroscopic ellipsometry. The center wavelength of the filters was obtained through spectral transmission measurement. The results suggest that the wavefront distortion of the multilayer coatings is dominated by the compressive stress of the SiO(2) layers and can be controlled and corrected by the amount of plasma ion momentum transfer, substrate temperature, postdeposition annealing, and stress compensation via backside SiO(2) coating. Based on the understanding of the mechanical and optical properties, the wavefront correction technique enables us to satisfy stringent surface figure specifications.     

Untersuchung des Sputter‐Ätzens auf die Eigenschaften von PVD‐CrN Hartstoffschichten auf Magnesium AZ91hp

Investigating the Influence of the Sputter Etching Process on the Properties of PVD‐CrN Coatings on Magnesium Die Cast Alloy AZ91hp A common method prior to the PVD deposition is the sputter etching process of the substrate itself to clean the surface from adhesion products and to improve the coating adhesion. This report deals with the sputter etching of magnesium die cast alloy AZ91hp to investigate the influences on the coating‐substrate interface, the surface properties and the mechanical properties of PVD‐CrN hard coatings. The coating‐substrate interface of the Cr‐AZ91 coating systems was investigated with XPS and SIMS. Surface studies were carried out by high resolution electron microscopy and AFM. The characterization of the mechanical properties of the CrN‐AZ91 compound systems includes thickness, coating hardness and hardness depth profiles, coating adhesion, structure and residual stresses. Some properties show a strong dependency of the etching time, especially the mechanical properties and the coating roughness. Increasing etching times lead to an improvement of the coating quality.     

Hardness and indentation-induced damage of SiC-coated graphite

The hardness and indentation damage of chemical vapour-deposited SiC coating/graphite substrate composites have been studied. Experimental results indicate that hardness is a non-linear function of coating thickness, and is not significantly affected by the changes in the magnitude of the residual stresses in SiC coating. The size of indentation lateral crack, observed using optical microscopy, varies with coating thickness. Acoustic emission spectra show that thinner coatings suffer more extensive fracture as compared with thicker coatings.     

Deposition of PVD Coatings on different geometries and local characterization for reliable properties

Although the characteristics of PVD coatings in research and development papers are very promising, in the field of tribology the industrial application of these coating types is restricted to special market segments up to now: the deposition of hard coatings is state of the art on tools, whereas PVD coated machine components are quite rare. This is caused by the coatings profile of properties, the various surroundings and the demands for application reliability. The last aspect is the main topic of this contribution. Reliability is especially important for machine components, because tools may fail after relative short life time compared to machine parts. Besides this tools and the corresponding production equipment are designed for fast tool replacement in contrast to other machines, which should work without standstill and with a minimum of maintenance. Characteristics of coated systems must be guaranteed in practice theory and laboratory experiments have to show what is possible. On the one hand reproduction of the deposition process must be guaranteed to enter application fields with high demands for reliability, on the other hand characterization of coated systems must be standardized with admissible deviations for communication between coaters and users. These aspects are important for decisions concerning the use of coating substrate systems in tribology besides the topics of technical function. The present investigation shows main reasons for deviations in results of PVD coatings.     

大面积应用的RF-PECVD技术研究

本文探讨采用小电极与大面积基片相对移动的方法来制造大面积薄膜的可行性,提出了采用小电极等离子体源在大面积基片上移动工作的新方法,可用于沉积(或刻蚀)均匀大面积薄膜或根据需求设计的大面积上非均匀膜厚分布的薄膜,从原理上避免大电极带来的不均匀性.介绍了这种方法中由两个电极构成的等离子体增强化学气相沉积(PECVD)系统.分析了当电极移动时,电极与真空室壁相对位置发生变化时对等离子体参数的影响.我们发现当两个射频电极之间的相位差为定值时,等离子体的分布随电极与真空室壁的距离(极-地距)变化而变化.当极-地距小于80mm时,随极-地距的增加,等离子体的悬浮电位和基片的自偏压下降,离子密度变化不明显.当极-地距大于80mm时,等离子体的分布呈稳定状态,各参数变化不明显.采用PECVD方法镀制了大面积薄膜厚度呈均匀分布和非均匀分布的两种薄膜,提供了膜厚呈线性渐变和抛物线变化的两种薄膜样片,显示了该方法的灵活性和可行性.     

Air Suspension Coating for Multiparticulates

Fluidized bed systems are widely used in the pharmaceutical industry for production of core material and for film coating. Top spray coaters, evolving from the fluid bed dryers of nearly 40 years ago, produce batches of fine, coated particles in excess of 500 kg. Wurster bottom spray equipment is used to manufacture pellets as well as to coat products ranging from powders to tablets. Rotary tangential spray systems generate micro pellets (approximately 100-600 microns) from powders, macro pellets (about 700-2000 microns) by layering, and apply coatings for all types of release. For all processes, films may be applied using water, organic solvents, or via hot melt to provide sustained or controlled release, taste masking, enteric release, improved stability, or aesthetics. However, depending on the type of substrate and coating material, the air suspension method selected may be a significant process variable. In addition to formulation considerations in product development, an understanding of these types of processing techniques is essential.     

Application of in situ ellipsometry in the fabrication of thin-film optical coatings on semiconductors

Thin-film interference filters, suitable for use on GaAs- and InP-based lasers, have been fabricated by use of the electron-cyclotron resonance plasma-enhanced chemical vapor deposition technique. Multilayer film structures composed of silicon oxynitride material have been deposited at low temperatures with an in situ rotating compensator ellipsometer for monitoring the index of refraction and thickness of the deposited layers. Individual layers with an index of refraction from 3.3 to 1.46 at 633 nm have been produced with a run-to-run reproducibility of 0.005 and a thickness control of 10 A. Several filter designs have been implemented, including high-reflection filters, one- and two-layer anitreflection filters, and narrow-band high-reflection filters. It is shown that an accurate measurement of the filter optical properties during deposition is possible and that controlled reflectance spectra can be obtained.     

High Velocity Oxy Fuel Spraying of Cold Work Tool Steels‐ A Novel Approach to Thick Coatings for Wear Protection Applications

Within this work, HVOF sprayed coatings based on X220CrVMo13‐4 cold work steel were applied to a S235JR construction steel substrate. The investigations focus on the influence of particle size and spray parameters on the coating microstructure, analyzed by means of optical microscope (OM) and scanning electron microscopy (SEM). Additional XRD measurements and micro hardness plots across the interface between substrate material and coating were carried out. Furthermore, the influence of particle size on the detected phases and coating porosity was studied. The results were compared with an X220CrMoV13‐4 reference sample produced by HIP.     

Effect of temperature on the growth of TiO2 thin films synthesized by spray pyrolysis: Structural, compositional and optical properties

Large surface area coatings of oxygen deficient nanocrystalline TiO₂ are of immense use in antifogging mirrors and self cleaning windows. Spray pyrolysis is a simple versatile technique to coat relatively large surface area. A clear understanding of effect of substrate temperature on the coating morphology, structure, composition and optical properties is essential to produce coatings of desired properties. Oxygen deficient nanocrystalline anatase–TiO₂ thin films were synthesized on Si(1 0 0), quartz and glass substrates at 300–550 °C. Well defined platelets like nanograins standing on their edge were obtained at 500 °C. The crystallites were found to be of ∼12 nm thickness and ∼30 nm major diameter. The secondary ion mass spectrometric studies of the films revealed uniform distribution of titanium and oxygen across the thickness of the film up to the film–substrate interface. Presence of lower valent Ti ions and oxygen vacancies were confirmed from XPS studies. The indirect and direct band gap values evaluated from the Tauc plot for films synthesized at 500 °C are 3.3 and 3.62 eV respectively.     

Air Suspension Coating for Multiparticulates

Abstract

Fluidized bed systems are widely used in the pharmaceutical industry for production of core material and for film coating. Top spray coaters, evolving from the fluid bed dryers of nearly 40 years ago, produce batches of fine, coated particles in excess of 500 kg. Wurster bottom spray equipment is used to manufacture pellets as well as to coat products ranging from powders to tablets. Rotary tangential spray systems generate micro pellets (approximately 100–600 microns) from powders, macro pellets (about 700–2000 microns) by layering, and apply coatings for all types of release. For all processes, films may be applied using water, organic solvents, or via hot melt to provide sustained or controlled release, taste masking, enteric release, improved stability, or aesthetics. However, depending on the type of substrate and coating material, the air suspension method selected may be a significant process variable. In addition to formulation considerations in product development, an understanding of these types of processing techniques is essential.