In‐situ Messung dünner Schichten auf Architekturglas

For the deposition of modern coatings on architectural glass (energy‐saving, solar control, anti‐reflective), reactive magnetron sputtering plays an outstanding role. The production of these coatings by reactive sputtering requires a manufactoring equipment, that ensures high quality as well as efficient deposition of the coatings. Thin film measurement by in‐situ ellipsometry can very impressively used for monitoring and controlling the film properties, in particular in the case of more complex coatings. With regard to long‐term stability the in‐situ film measurement is of special importance with respect to the use of the novel mid‐frequency magnetron sputter technique. This technique allows the deposition rate to be increased up to 500 %, however, a dynamical plasma stabilization in the so called »transition mode« is necessary. Within the framework of a project supported by the BMBF, the spectroscopic ellipsometry was implemented on a large scale glass deposition plant (Semco Glasbeschichtung, Neubrandenburg) and was tested during the production. The investigations show that ellipsometry is outstandingly suitable for an accurate determination of the optical layer properties of coatings on architecture glass, even for complex layer systems. Therefore, the basis for an improvement of the efficiency of the plant is given.     

In situ optical characterization and reengineering of interference coatings

A new optical monitoring system has been developed that allows recording of transmission spectra in the wavelength range between 400 and 920 nm of a growing optical coating during deposition. Several kinds of thin film sample have been prepared by use of a hybrid monitoring strategy that is essentially based on a combination of quartz monitoring and in situ transmission spectra measurements. We demonstrate and discuss the applicability of our system for reengineering procedures of high-low stacks and measurements of small vacuum or thermal shifts of optical coatings.     

Vakuumbeschichtung von PET‐Folie mit Solar‐Control‐Schichten

Solar control coatings as an integrated part of automotive glass are increasingly used in a growing number of car models of all classes of the European car manufactures. The advantages of that solar control laminated glass are an increased reflection in the near infrared spectral region, which results in a reduction of heat gain of about 50 % in the cabin caused by solar radiation, an increase of passenger comfort and the safe of fuel for air conditioning. One process for the production of solar control coatings is the magnetron sputtering onto optical grade flexible PET‐film. The performance of these coatings as well as technological issues of the deposition process are presented.     

Hartstoffschichten für das Pressen und Prägen von Gläsern bei hohen Temperaturen

Hard and wear resistant coatings for the moulding and embossing of glasses at elevated temperatures Hard and wear resistant coatings of Titanium Aluminium Nitride TiAlN were deposited on various substrates by the application of different reactive deposition processes: RF-magnetron-sputtering, ion beam-sputtering and by the energetic cluster impact (ECI) process. The deposition of the coatings was performed under variation of biasing conditions and of process parameters such as pressures and flow rates of the process gases argon and nitrogen as well as of energies of species hitting the substrate surfaces. The microstructure particularly the growth morphology of several films was investigated by pictures of film cross sections recorded by transmission electron microscopy. Residual intrinsic film stresses were analyzed by measuring deflections of substrates in an interference optical microscope before and after the deposition of the coatings. By heating coated substrates and in-situ observation of deflections at elevated temperatures dependencies of thermally induced stresses on temperatures and variations of intrinsic stresses due to changes within the films could be analyzed and related to microstructure and growth conditions. In the paper specific characteristics of the deposition processes occuring on the scale both of atoms and of clusters which may contain several thousand of atoms are described and related to microstructure, residual stress states and damaging conditions. Different contributions to residual film stresses are analyzed on the base of theoretical considerations taking into account deposition kinetics and thermomecanical properties. The significance of achieved film properties for application, i. e. for the coating of tools for the manufacturing of optical components by moulding and embossing of glasses is discussed.     

Realistische Modellierung der NIR/VIS/UV‐optischen Konstanten dünner optischer Schichten im Rahmen des Oszillatormodells

Modelling the NIR/VIS/UV optical constants of thin solid films: An oscillator model approach Based on a multioscillator approach, we demonstrate the determination of optical constants of different optical coating materials. The advanced LCalc‐software allows calculating the dielectric function as well as refractive index and extinction coefficient through a fit of transmittance and reflectance spectra measured at one or several angles of incidence. Sufficiently accurate spectrophotometric measurements are carried out by means of self‐developed VN‐ The thus obtained optical constants are automatically Kramers‐Kronig‐consistent and in reasonable correspondence to various kind of side information available about the coatings. This is demonstrated for dielectric oxide coatings as well as for one transparent conductive oxide (ITO) and a metal layer (aluminium). In application to reproducibility experiments, the method allows estimating process‐inherent stochastic variations in optical constants, which represent themselves an essential input for advanced computational manufacturing runs for design optimization prior to deposition.     

Simple Method for Determining Slowly Varying Refractive-Index Profiles from in situ Spectrophotometric Measurements

Reliable control of the deposition process of optical films and coatings frequently requires monitoring the refractive-index profile throughout the layer. In the present research a simple in situ approach is proposed that uses a WKBJ matrix representation of the optical transfer function of a single thin film on a substrate. Mathematical expressions are developed that represent the minima and the maxima envelopes of the curves transmittance versus time and reflectance versus time. The refractive index and the extinction coefficient depth profiles of different films are calculated from simulated spectra as well as from experimental data obtained during the PECVD (plasma-enhanced chemical vapor deposition) of silicon-compound films. Variation in the deposition rate with time is also evaluated from the position of the spectra extrema as a function of time. The physical and mathematical limitations of the method are discussed.     

Laser treatment of optical Nb2O5‐ and HfO2‐films

Optical thin films have to fulfil high quality requirements, which can be achieved for example by reactive low voltage ion plating (RLVIP). But especially for applications in precision optics, additional treatments are necessary to reduce residual optical absorption and compressive stress arising in the coatings, and to enhance the stability of the coatings – specifically for laser applications. In practice, post deposition heat treatment and backside coatings are mostly used to overcome these problems. In order to provide alternative methods to handle the disadvantages of the RLVIP‐process, the idea was to replace the mentioned steps by a laser treatment. This means that a laser beam is directed onto the sample after deposition or even during the coating process. In this study, the influence of a high power CO²‐laser beam on thin Nb²O⁵‐ and HfO²‐films was investigated. The effects on the refractive index and the film thickness are presented for different energy densities of a TEA‐CO²‐laser beam (10.59μm). For Nb²O⁵‐films a thickness increase up to 12.2nm (6.4 %) and a refractive index decrease of 0.074 (3.1 %) were found. In case of HfO² the values were 2.3nm (1.2 %) in thickness and 0.007 (0.3 %) in refractive index. From the observed changes also distinct impacts on the film stress can be expected. One intention of this research was also to call attention to an alternative technique for enhancement of thin film properties.     

Herstellung von Polymer‐ und Polymer‐Metalloxid‐Kompositschichten

Preparation of polymer and polymermetal oxide composite thin films Organic materials are not yet commonly used for optical interference layer systems. The reasons therefor are their low mechanical resistivity, their often more complex deposition techniques and their poorer optical properties compared with oxide thin films. However some organic materials offer special properties that are useful for the application in optical layer systems. Because of its high mechanical flexibility mechanical stress in layer systems can be reduced. Some organic materials show specific optical properties like fluorescence or intensive colors that can be used for optical layer systems. Hydrophilic and hydrophobic organic top coatings can improve the pollution behavior of optical layer systems. Therefore we present in this work some gas phase deposition techniques for organic substances and report about some basic optical and mechanical properties of thin films coated with these as well as some important process characteristics.     

Magnetron sputter‐deposition on atom layer scale

For many applications there is an increasing request to control the deposition process on an atom layer scale. This offers a lot of advantages like in accuracy, layer homogeneity and tailoring of layer properties. On the other hand the speed and throughput of the process should not suffer from the control on an atom layer scale as it is the case for classical atom layer deposition (ALD). For optical applications especially high‐end interference filter coatings we developed a plasma assisted reactive magnetron sputtering process in combination with a high speed drive for the substrates. This combination allows controlling the layer thicknesses and layer properties on an atom layer scale while maintaining a high deposition rate. The advantages of this process are demonstrated on single layer results of SiO2, HfO2, ZrO2, Ta2O5 and mixed oxides of SiO2‐Nb2O5. Morphology, surface roughness, film stress, refractive index and losses are controlled by the oxygen partial pressure, the substrate temperature, the energy input by the sputtering ‐and assist process and by cosputtering. The outstanding performance of high‐end interference filter coatings like a multi notch filter for fluorescence microscopy is achieved by the very stable and reproducible deposition process in combination with an advanced thickness control strategy based on in‐situ optical thickness control and time control.     

UV‐verstärkte Silberschichten

UV‐enhanced Ag‐coatings with optimized environmental stability For the construction of optical instruments, mirrors with silver (Ag) coatings are of great importance, because Ag has the highest reflectivity of all metals from the visible (VIS) throughout the infrared (IR) spectral range. Investigations performed at IOF show, that the deposition of a closed and dense protective layer is a necessary but not a sufficient condition for the effective protection of silver: hygroscopic particles can harm even silver coatings protected by a previously defect‐free protective layer. In order to improve the protection, a nanolaminate approach for Ag‐protection has been developed. By this approach, both the environmental stability and the optical performance can be optimized.     

Cold spraying of Cu‐Al‐Bronze for cavitation protection in marine environments

High strength metal coatings are promising for reducing the cavitation damage of ship rudders. Cold spraying offers the opportunity to produce coatings that have similar properties as respective bulk material. In this study, conditions for cold spraying CuAl10Fe5Ni5 bronze are evaluated for the use at ship rudder applications. The spray parameter sets were varied with respect to nozzle type, process gas pressure and temperature. Single particle impact morphologies were investigated by scanning electron microscopy and categorized into different classes to obtain information on the deformation behavior. Within the selected parameter regime, coatings were processed with deposition efficiencies of up to 70%. The coating microstructures were analyzed by optical microscopy to gain information on spraying conditions for minimum porosity. For the higher parameter sets, porosities of less than 2% were obtained. Coating performance was investigated by cavitation test procedures. These first results show that cold sprayed bronze coatings still faces challenges with respect to powder properties. With further optimization, respective coatings could have a high potential for ensuring a good performance in rudder protection.     

Reactive Low Voltage Ion Plating (RLVIP). Prozess‐, Plasma‐ und Schichteigenschaften am Beispiel von Ta2O5/SiO2

Reactive Low Voltage Ion Plating (RLVIP) is a process for production of chemical compound films mainly by direct synthesis from the elements. It can be used for deposition of single layer and multilayer oxide coatings onto unheated glass and other unheated substrates. An introduction to the RLVIP process will be given, together with some relevant plasma process data and optical and mechanical film properties of Ta₂O₅ films and Ta₂O₅/SiO₂ multilayers. The process plasma was analysed by plasma monitoring (PPM421), a Langmuir probe system (Smartprobe) and a Faraday Cup System (MIEDA). A correlation between plasma data and optical/mechanical properties will be shown.     

Abscheidung optisch,elektrisch und akustisch wirksamer Schichten mit dem Doppel‐Ring‐Magnetron

Numerous applications in optics, electronics and sensor technology require thin dielectric films. Conventionally they are deposited by evaporation, activated evaporation, rf‐sputtering or CVD‐techniques. This paper describes the deposition of such films using reactive Pulse Magnetron Sputtering. This technology not only enables a tenfold deposition rate compared to the conventional techniques but also offers new possibilities for influencing film growth. For example it is possible to alter film composition during deposition and hence to deposit complete optical systems without interruption of the plasma process. Furthermore the energetic bombardment of the growing film can be controlled in a wide range by the pulse mode and the pulse parameters. This can be used to either deposit very dense films by strong energetic bombardment or to deposit films at low thermal load onto temperature sensitive substrates. Examples of film deposition for laser optics, electrical insulation applications and surface acoustic wave devices show how these new technological possibilities advantageously can be used for creating innovative layer systems. Film deposition is carried out in stationary mode using a Double Ring Magnetron. This type of magnetron ensures film thickness uniformity better than ± 1 % on 8” substrates by the superposition of the thickness distributions of two concentric discharges.     

Optical properties of pulse laser deposited AlN thin films on silicon

Aluminium-nitride thin films were deposited on silicon Si(111) substrate with pulsed laser deposition in a Riber LDM-32 system. The optical properties of the films were studied by means of optical spectroscopy with an incoherent light source mainly covering the visible range. It is demonstrated that, in comparison with an aluminium mirror, under certain deposition conditions, the film may behave as a metallic thin film as far as the optical reflection is concerned. In this case, there is an enhanced plasmonic reflection peak in the optical spectrum and the peak may be modified according to the degree of the phase transition. The microscopic structures as well as the surface topographies of the films were also studied with X-ray photoelectron spectroscopy and scanning electron microscopy. It turns out that the density and the size of the microscopic domains in the film determine whether the film remains dielectric or becomes metallic. The diamagnetic effect in the enhanced plasma increases in the process when the sample is smoothed out with the optimized nitrogen gas pressure. The nitrogen pressure is thus identified as the most influential deposition condition to the phase transition.     

Neuartige dekorative Farbschichten durch Plasma‐Beschichtung

Novel decorative color coatings using plasma deposition The market does not stop to demand for novel products. Only those who offer innovative products will explore new segments of the market and will not loose against the cheap suppliers from far eastern countries. This is even more important in the field of surface technology. Many products would not be competitive without plasma technology. Companies changing surfaces with plasma technology expect a noticeable growth between 20 and 50 % within the next years [1]. The deposition of thin layers using plasma makes it possible to obtain highly brilliant color coatings, specially mixed color effects (rainbow like) as well as color changes depending of the observation angle. These optical special effects would not be feasible with common painting techniques. Thus plasma deposition opens a new field for surface coating. In these layers the colors are created via interference effects of the light being used for illumination. They are called interference colors, well known to the most of us from thin oil films on a wet street.     

Anforderungen an Beschichtungen für den optischen Gerätebau

Demands on Coatings for Optical Devices Growth in optical technologies requires reliable optical equipment composed in important parts by high quality optical thin film components. Outstanding performance in coatings is an essential demand for optimum functionality and overall stability of the optical apparatus. Developmen of new / hybrid film deposition techniques for industrial use and search for new materials and improved film system design are strictly required.     

Influence of deposition conditions on optical properties of aluminum nitride (AlN) thin films prepared by DC-reactive magnetron sputtering

Aluminum nitride (AlN) films have been prepared by DC-reactive magnetron sputtering technique. The optical properties of the films have been studied by optical spectroscopy with an incoherent light source. For the first time, it is demonstrated that for certain deposition conditions, the film may behave as a metallic thin film. In this case, there are strongly enhanced reflection peaks in the optical spectrum and the peaks may red-shift according to the degree of the metallization. The microscopic structures of the films have also been studied with scanning electron microscopy (SEM) and X-ray diffraction (XRD). It turns out that the orientation of the crystallites in the film determines whether the film remains dielectric or becomes metallic. It is found that the degree of the metallization depends on the proportion of (1000) preferred orientation in the film. In the deposition process, various deposition parameters have been experimented and a close relation between the deposition parameters and the status of the films is established. The most influential deposition conditions are as follows: the substrate temperature in a range from 200 to 700 °C, the gas composition ratio of Ar/N₂ from 20/80 to 60/40 and the plasma current from 0.2 to 0.45 A.     

Imaging reflectometry in situ

An innovative method of in situ real-time optical monitoring of thin film deposition and etching is presented. In this technique, intensity maps of a thin film corresponding to a series of wavelengths selected by a monochromator (300-800 nm) are recorded by a CCD camera. From the maps the reflectance spectra at individual points of the sample surface can be extracted. By fitting the reflectance spectra to the theoretical ones, the maps of a thin film morphology (including optical parameters) and their temporal development during technological processes can be obtained. The method was tested by in situ observation of the growth of silicon nitride and silicon oxide thin films prepared by ion beam sputtering and by the monitoring of etching of thermally grown SiO(2) thin films.     

PVD‐Schutzschichten für Werkzeuge des Präzisionsblankpressens

PVD protective coatings for precision molding tools Precision glass molding (PGM) is a replicative hot forming process for the production of complex optical components, such as aspherical lenses for digital and mobile phone cameras or optical elements for laser systems. The efficiency and thus also the profitability of the PGM depend on the unit price per pressed component, which correlates primarily with the service lifetime of the pressing tools. To increase tool lifetime, the tool surfaces are coated with protective coatings based on precious metals or carbon using physical vapour deposition (PVD). The PVD coating technology enables the deposition of thin coatings, which also follow more complex surface geometries and achieve a high surface quality. PVD coatings are also commonly used to protect tools from wear and corrosion. This paper presents two chromium‐based nitride hard coatings produced by an industrial PVD unit and investigated for their applicability for PGM. Two different coating architectures were implemented, on the one hand a single coating chromium aluminium nitride (Cr,Al)N coating and on the other hand a nanolaminar CrN/AlN coating with alternating layers of chromium nitride and aluminium nitride. The latter is a coating consisting of hundreds of nano‐layers, only a few nanometers thick. Both coatings, (Cr,Al)N and CrN/AlN, each have a thickness of s ～ 300 nm in order to follow the tool contour as closely as possible. The properties of the coating systems, which are of particular relevance for PGM, are considered. These include on the one hand the adhesion of glass, the roughness and topography of the surface and the adhesion between the coating and the tool material. In addition, the barrier effect of the coatings against diffusion of oxygen was investigated. In order to reproduce the thermal boundary conditions of the PGM, thermocyclic aging tests are performed and their influence on the different properties is described.