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.     

含钛MoS2合金减摩镀层摩擦学性能研究

应用闭合磁场非平衡磁控溅射离子镀技术,制备了不同Ti含量的MoS2合金减摩镀层,研究了添加元素Ti含量对镀层厚度、硬度、摩擦系数等的影响规律.结果表明MoS2合金减摩镀层的厚度与添加元素Ti溅射靶的输入功率无关,其硬度随Ti含量增加而提高.不同Ti含量的镀层摩擦系数呈现出不同的变化规律.Ball-on-disc 球盘摩...     

Fabrication of High Performance Laminated Polarization Splitters Consisting of Thick a-Si:H /SiO(x):H Multilayers

We report fabrication techniques ofa-Si:H/SiO(x):H multilayers having ample thickness and flat layer boundaries for high performance laminated polarization splitters (LPS's). In the new fabrication process we used the following techniques to achieve low stress and high surface flatness: SiO(x):H film deposition by rf sputtering with a mixture of Ar/H(2), two-step deposition using rf bias sputtering, and elimination of surface roughness and defects by mechanical polishing. This process enabled deposition of a multilayer as thick as 265 mum while preserving layer boundaries as flat as 1 nm (rms). As a result, LPS's having low loss, a large aperture, and a long splitting distance were successfully obtained. The high optical performance is applicable to functional devices integrated into fibers or planar waveguides.     

Mechanical properties optimization of tungsten nitride thin films grown by reactive sputtering and laser ablation

Transition metal nitrides coatings are used as protective coatings against wear and corrosion. Their mechanical properties can be tailored by tuning the nitrogen content during film synthesis. The relationship between thin film preparation conditions and mechanical properties for tungsten nitride films is not as well understood as other transition metal nitrides, like titanium nitride. We report the synthesis of tungsten nitride films grown by reactive sputtering and laser ablation in the ambient of N₂ or N₂/Ar mixture at various pressures on stainless steel substrates at 400  C. The composition of the films was determined by XPS. The optimal mechanical properties were found by nanoindentation based on the determination of the proper deposition conditions. As nitrogen pressure was increased during processing, the stoichiometry and hardness changed from W₉N to W₄N and 30.8-38.7 GPa, respectively, for films deposited by reactive sputtering, and from W₆N to W₂N and 19.5-27.7 GPa, respectively, for those deposited by laser ablation.     

Correlation between structure and optical properties in low emissivity coatings for solar thermal collectors

We have investigated the relation between the structure and morphology of TiN coatings with their optical properties. Samples were deposited by magnetron sputtering and, by changing the deposition parameters, different textures and chemical compositions can be obtained as measured by X-ray diffraction and glow discharge optical emission spectroscopy respectively. The transmittance in the visible range, measured by spectroscopic ellipsometry, and the emittance, derived from reflectance in the far infrared range as measured by Fourier Transform Infrared Spectroscopy have been related to the nitrogen atomic content and the preferred crystalline orientations present in the TiN coatings. The visible transmittance of the coatings was found not to be dependent on the preferential orientation, while the emittance clearly improves with increasing the film thickness and the presence of both (111) and (200) crystal orientations.     

Advanced key technologies for magnetron sputtering and PECVD of inorganic and hybrid transparent coatings

Besides classical multilayer systems with alternating low and high refractive indices, reactive pulse magnetron sputtering processes offer various possibilities of depositing gradient films with continuously varying refractive index. Using nanoscale film growth control it is possible to achieve optical filter systems with a defined dependency of refractive index on film thickness, e.g. by sputtering a silicon target in a time variant mixture of oxygen and nitrogen. Also reactive co-sputtering of different target materials such as silicon and tantalum in oxygen is suitable as well. Rugate filters made from SiO_xN_y or Si_xTa_yO_z gradient refractive index profiles find their application in spectroscopy, laser optics and solar concentrator systems.Furthermore polymer substrates are increasingly relevant for the application of optical coatings due to their mechanical and economical advantages. Magnetron PECVD (magPECVD) using HMDSO as precursor allows to deposit carbon containing films with polymer-like properties. Results show the suitability of these coatings as hard coatings or matching layers. Multifunctional coatings with antireflective and scratch-resistant properties were deposited on polymer substrates using a combined magPECVD and sputter deposition process.     

柱弧离子镀和非平衡磁控溅射镀制备Ti-N-C黑色硬质膜

采用柱弧离子镀和中频孪生靶非平衡磁控溅射镀膜技术制备了Ti-N-C多层复合黑色硬质膜.采用轮廊仪扫描电子显微镜(SEM)、分光光度计、显微硬度计等手段研究了所得膜层的各项性能.结果表明,两种工艺都可以获得颜色较深的黑色硬质膜,柱弧离子镀制备黑色硬质膜的效率高、力学性能更好;中频孪生靶非平衡磁控溅射制备的黑色硬质膜表面光滑、颜色更深.     

Micro-scratch analysis and mechanical properties of plasma-deposited silicon-based coatings on polymer substrates

Advanced optical applications require multifunctional coatings with specific mechanical properties, such as resistance to damage and good adhesion to different types of substrates, including polymers. In the present study we deposited amorphous hydrogenated silicon nitride (SiN_1.3) and oxide (SiO₂) films on polycarbonate and on silicon substrates by plasma enhanced chemical vapor deposition (PECVD), using a dual-mode microwave/radio frequency plasma system. The film adhesion was determined by the micro-scratch test. Depth-sensing indentation and substrate curvature measurements were used to evaluate the microhardness. Young's modulus and residual stresses of the films. The adhesion strength, represented by the critical load, L_c, when the film starts to delaminate, was determined as a function of the substrate material and the energy of bombarding ions. A direct correlation between the L_c values and the mechanical properties of the films was found. The formation of different crack patterns in the coatings during the scratch procedure is explained in terms of stress release mechanism depending on the mechanical properties of the film, the substrate and the interface region. In addition, different models applicable to the evaluation of the work of adhesion in the case of hard coatings on soft substrates are critically reviewed.     

Spectroscopic ellipsometry and positron annihilation investigation of sputtered HfO2 films

Hafnium oxide (HfO₂) films were prepared using a pulsed sputtering method and different O₂/(O₂ + Ar) ratios, deposition pressures, and sputtering powers. Spectroscopic ellipsometry (SE) and positron annihilation spectroscopy (PAS) were used to investigate the influence of the deposition parameters on the number of open volume defects (OVDs) in the HfO₂ films. The results reveal that a low O₂/(O₂ + Ar) ratio is critical for obtaining films with a dense structure and low OVDs. The film density increased and OVDs decreased when the deposition pressure was increased. The film deposited at high sputtering power showed a denser structure and lower OVDs. Our results suggest that SE and PAS are effective techniques for studying the optical properties of and defects in HfO₂ and provide an insight into the fabrication of high-quality HfO₂ thin films for optical applications.     

准晶薄膜与涂层的制备、性能和应用

本文综述了近年来准晶薄膜的制备方法、性能及其应用等方面的研究工作。准晶薄膜的制备方法主要有物理汽相沉积法和热喷涂法两大类。准晶薄膜具有优异的力学、热学与光学等性能,已经应用于不粘锅涂层、热障涂层和太阳能吸收器等。     

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.     

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.     

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.     

Deposition of functional coatings on polyethylene terephthalate films by magnetron-plasma-enhanced chemical vapour deposition

Magnetron-plasma enhanced chemical vapour deposition (PECVD) is a process tool which allows the deposition of plasma polymer coatings at process pressures below 1 Pa. The striking features of this technology are the relatively easy realisation of large area deposition as well as the possibility of the combination with sputtering processes for multilayer coating designs. SiO_xC_y coatings were deposited on polymer film in a roll-to-roll deposition machine. Dynamic deposition rates as high as 120 nm?m/min were achieved. The process was set up with both the monomer hexamethyldisiloxane and the monomer tetraethylorthosilicate (TEOS) and with mixtures thereof. The coatings were analysed by Fourier transform infrared spectroscopy. This method identifies the existence of different types of Si-O bonding in the layer. The results show how the layer properties are linked to the plasma parameters of the deposition process. The properties were compared to sputtered SiO₂ and to layers obtained by other PECVD processes. Elastic recoil detection analysis (ERDA) was used in order to determine the composition of the samples. Both IR spectroscopy and ERDA revealed that the usage of TEOS provided more SiO₂-like layers. The process was applied to the deposition of optical multilayer coating in a roll-to-roll coating system.     

Mechanical properties of CN<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> coatings obtained by carbon arc sputtering

Internal stresses σ₀, friction coefficients fand microhardness were measured in diamond-like coatings obtained by vacuum-arc sputtering of carbon target at different nitrogen pressures in a work chamber during deposition on metallic substrates. The dependence of these parameters on nitrogen concentration in coatings can be used in practical deposition of strengthening and friction coatings for improvement of their tribological properties. The correlation between mechanical properties of diamond-like and CN _x coatings was established.     

Gasochromic switching of reactively sputtered molybdenumoxide films: A correlation between film properties and deposition pressure

Molybdenumoxide (MoO_x) thin films can change their optical properties upon exposure to hydrogen. Since the film properties strongly depend on process parameters we have studied how the films are affected by the total pressure during deposition. Stoichiometric and sub-stoichiometric MoO_x films were prepared by reactive direct current magnetron sputtering in an atmosphere of argon and oxygen. Substoichiometric films were coated with platinum as a catalyst and were colored in diluted hydrogen atmosphere and bleached in air. Optical spectroscopy, X-ray reectometry, spectroscopic ellipsometry and simulations of the measured spectra were used to characterize the films ex situ. In situ switching characteristics as revealed by optical spectroscopy and changes in stress were measured as well. We find that the total pressure during sputter deposition has a strong influence on the optical constants, the film density, and the sputter rate. The mechanical stresses and switching Preprint submitted to Elsevier Science 10 March 2006 cycles during the film coloration and bleaching also strongly depend on the total pressure. The influence of the sputter pressure on film properties is explained by the kinetics during the sputter process.     

Control of the optical properties of silicon and chromium mixed oxides deposited by reactive magnetron sputtering

The development of mixed-oxide thin films allows obtaining materials with better properties than those of the different binary oxides, which makes them suitable for a great number of applications in different fields, such as tribology, optics or microelectronics. In this paper we investigate the deposition of mixed chromium and silicon oxides deposited by reactive magnetron sputtering with a view to use them as optical coatings with an adjustable refractive index. These films have been characterized by means of Rutherford backscattering spectrometry, Auger electron spectroscopy, X-ray diffraction, scanning electron microscopy, Fourier-transform infrared spectroscopy and spectroscopic ellipsometry so as to determine how the deposition conditions influence the characteristics of the material. We have found that the deposition parameter whose influence determines the properties of the films to a greater extent is the amount of oxygen in the reactive sputtering gas.     

Growth defects in PVD hard coatings

In PVD coatings, various growth defects typically appear during the deposition. Such defects are drawbacks in coating application. In order to improve the tribological properties of PVD hard coatings it is important to minimize the defect density. Various PVD hard coatings were prepared by evaporation using a thermionic arc and by sputtering using unbalanced magnetron sources. Coating topography was analyzed using a 3D stylus profilometer and other analytical techniques (SEM, FIB). We studied the influence of different types of substrate materials, the substrate position in the vacuum chamber, pre-treatment and deposition parameters on defect density.     

Ion-beam etching for the precise manufacture of optical coatings

We propose using ion-beam etching as an additional tool for the accurate control of the thickness of thin films during the manufacture of sensitive optical multilayer coatings. We use a dual ion-beam sputtering system in the deposition and etch modes. In the deposition mode both the assist and sputtering ion beams are used to produce dense films at deposition rates in the range of 0.1-0.3 nm/s. In the etch mode, only the assist ion beam is used to remove material at a rate of less than 0.1 nm/s. A very high precision in the layer thicknesses can be obtained by alternating between deposition and etch modes. We observed that etching did not significantly affect the surface quality and the uniformity of the coatings. We introduced etching into our current manufacturing process and demonstrated its potential for the fabrication of several optical multilayer systems with performances that are very sensitive to the thickness of their layers.     

Properties of amorphous carbon films deposited by ion beam methods

Amorphous carbon films were prepared by the ion beam sputtering of graphite, by the ion beam sputtering of graphite with simultaneous ion bombardment of the growing film, and by primary ion beam deposition using a beam from a methane- argon plasma. The films are semiconducting in nature, having band gaps of the order of 1 eV. A nuclear reaction involving an energetic (2 MeV) beam of ¹¹B⁺ was used to obtain hydrogen profiles of the films. It was found that the electrical, optical and mechanical properties of the films could be correlated with the hydrogen content. The observed properties are explained qualitatively in terms of amorphous semiconductor theory.