Proceedings Volume 5963

Advances in Optical Thin Films II

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Proceedings Volume 5963

Advances in Optical Thin Films II

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Volume Details

Date Published: 30 September 2005
Contents: 13 Sessions, 76 Papers, 0 Presentations
Conference: Optical Systems Design 2005 2005
Volume Number: 5963

Table of Contents

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Table of Contents

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  • Invited Session
  • Design
  • Filters
  • Monitoring
  • DUV/VUV Coatings I
  • DUV/VUV Coatings II
  • XUV Coatings
  • Radiation Resistant Coatings
  • Manufacturing I
  • Manufacturing II
  • Manufacturing III
  • Poster Session
  • Additional Paper from Session on XUV Coatings
Invited Session
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Milestones in optical coating technology-from A. Smakula/John Strong until today
The first optical interference coatings were produced about 70 years ago. Since then, the optical coating industry has grown to serve a $2.1 billion market worldwide. There are three requirements to produce good multilayer optical interference coatings: 1. a good theoretical design; 2. at least two reliable coating materials; and 3. production processes which allow the deposition of these materials. A chart of historic milestones in the design of optical coatings was published before (An updated version of this chart is given below). In this paper we make an attempt to develop a similar chart of milestones in optical coating technology (harder, more stable and moisture resistant coating materials) and better production processes (more reliable, more precisely monitored, and allowing large area/high volume deposition).
Antireflection coatings: key optical components
The topic of antireflection coatings is vast, and it is impossible to review it comprehensively in an article of this size. Here an attempt is made to show how antireflection coatings evolved from inhomogeneous layers, through homogeneous layers with optical thicknesses that were multiples of a quarter wave of some central wavelength, to the modern non-quarter wave designs that, at times, may consist of many tens of layers. Antireflection coatings for the solution of a number of special problems are presented.
Design
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New optimization algorithm for the synthesis of rugate optical coatings
By comparing multilayer and rugate solutions to a typical rugate synthesis problem we demonstrate that rugate synthesis methods are still of a great importance. The new accurate algorithm for the synthesis of rugate coatings with arbitrary refractive index profiles is discussed. It is shown that this algorithm can be successfully applied for solving such classical rugate synthesis problem as reducing sidelobes accompanying stopbands of rugate filters.
Colorimetry in optical coating
Generally, the colour of the non-luminous objects in nature is due to absorption, diffusion and refraction of light. The colour of the optical coatings, as that of some kind of bird feathers, soap bubbles, butterfly wings, some insects, etc. is due to interference and therefore is named interference colour. This kind of colour belongs to the gonio-apparent or special-effect colours. Generally, industrial colorimetry does not deal with interference colour and the usual colorimetric instruments are inadequate to measure it. Only recently, with the new mica-pigment coatings, colorimetry is considering the measurement of the interference colour and new multiangle spectrophotometers are produced. This work is a general introduction to the ground of colorimetry and, at the end, deals with interference colours. A short overview is given of the Physiological Optics and of the Colorimetric Standards of the "Commission International de l'Eclairage" (CIE): particularly, Psychophysical Colorimetry, Psychometrical Colorimetry and Measurement Geometries are summarised. The colorimetry of gonio-apparent colours is considered. For a complete and detailed optical characterisation of interference colour the measurement of bidirectional transmittance and reflectance is needed. Particularly, basic elements for the colorimetric analysis of the interface between isotropic non-absorbing media and for thin monolayers are given.
Fourier Transform estimation of reflecting thin film thickness
A parallel was recently established between an empirical procedure for the estimation of reflecting thin film thickness and new results derived from a Fourier Transform (FT) thin film synthesis technique. For simplicity the proposed FT approach was limited to a particular case. The approach is generalized in the present work and practical considerations are discussed. It is shown that good results are possible although the generalized problem is more complex from the FT point of view.
Thin-film coatings and transmission-polarization-devices: negative system
A. R. M. Zaghloul, M. Elshazly-Zaghloul
In this communication, we discuss the behavior of the negative transparent-film transparent-substrate film-substrate system as a transmission-polarization-device. A transmission-polarization-device is defined as a device that produces pre-specified polarization changes of the electromagnetic wave upon transmission through the device. A comprehensive account of all devices is presented through the analysis of the transmission polarization function of the film-substrate system. We present device-specific closed-form design formulae for each and every device. We also present a general-device design-formula to design any and all transmission-polarization-devices. In this communication, thin-film coatings are treated as polarization devices.
Filters
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Laser trimming of thin-film filters
The use of a photosensitive material for manufacturing the spacer of bandpass thin-film filters is a very attractive way for enabling the post-processing of such devices with the help of a light beam, either to correct with a high accuracy the consequences of some deposition errors on the filter properties (central wavelength out of specifications, inadequate spatial uniformity) or to create entirely new filtering devices with controlled spatial properties (for instance, variable filters with arbitrary profile). A theoretical presentation of the main problems arisen by such a laser trimming will be done, first for bandpass thin-film filters but also for multiple-cavity Solid Spaced Etalons (SSE). After a comprehensive analysis of the possible materials which can be selected for such an application, we will conclude our presentation by the description of the first experimental results obtained by our team in this new field, including a rapid presentation of the dedicated control means needed by this spatially localized approach of a filtering device.
Optical coatings for artwork preservation and enhanced viewing
A. Piegari, R. Arrighi, I. Di Sarcina, et al.
Many optical methods are nowadays in use in the field of art. Most techniques are applied for characterization of materials, monitoring, diagnostics. Optical thin films can find an interesting application for artwork protection from the damage induced by illumination. The deteriorating effect of light on artworks is well known and the conventional approach to reduce the damage consists in lowering the radiation intensity and shortening the exposure duration. A complementary approach is to block all radiations that are not useful for viewing the artwork. A proper optical coating deposited on glass is able to cut the radiation flux at all wavelengths outside the range of sensitivity of the human eye. Glass is already in use in museum and galleries to protect artwork from vandalism and the use of coated glass can result in a simple method for contributing to art conservation. The optical coating will also improve the viewing because of the antireflection effect that can be combined with the protection properties. Particular care must be taken of this aspect because a compromise between conservation rules and visitor satisfaction must be reached. It is important that the thin-film coating does not introduce color alterations from the point of view of the observer and for this reason color testing on coated glasses must be carried out with real viewers.
Steep-edge filter design with equivalent layers
Based on a special definition of the edge region of a thin-film interference filter, an approach to design steep-edge filters using the theory of equivalent layers is presented. Some features are discussed using the known theory to meet the topical filter requirements. An example is theoretically outlined and the spectral performance of a manufactured filter is presented.
Manufacturing of linear variable filters with straight iso-thickness lines
Laetitia Abel-Tiberini, Frédéric Lemarquis, Gérard Marchand, et al.
Linear variables filters are band-pass multilayer coatings manufactured with a thickness gradient that allows a significant wavelength shift of the centring wavelength of the filter according to the point that is illuminated. In case such a filter is associated with a 2D matrix detector in order to form a compact spectrometer, iso-thickness lines must be as straight as possible, perpendicularly to the thickness gradient. To answer this problem, we developed a masking mechanism that combine the classical rotation movement of substrates and a translation movement for the mask, this last movement being induced during the rotation by the mean of a cam. Thickness gradient can be freely adjusted according to specifications, while transverse uniformity is 99.9%.
Studies on superprism effects in multilayer thin film stacks
X. Liu, X. Z. Sun, P. F. Gu R.N.
The concept of "Superprism" which is used in photonic crystal will be introduced into optical thin film coatings, due to the fact that the group velocity of the light is different as the wavelength in certain special case for the multiplayer thin film coatings. In this paper, The "superprism" effect of multilayer thin film coatings will be presented both from theoretical analysis and experimental results, these researches will create an new application of the thin film coatings not only to be a spectral filter but also can acts as "thin film gratings".
Monitoring
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Substantial progress in optical monitoring by intermittent measurement technique
A. Zoeller, M. Boos, R. Goetzelmann, et al.
The production capabilities for optical multilayer coatings were improved significantly in the last decade. So called "shift free" coatings have become a standard in the coating production. Direct optical monitoring plays a key role to improve the layer thickness accuracy and takes advantage of error compensation effects. For the production of DWDM filters direct monitoring was introduced in the last decade. Continuous measurement is applied on relatively small substrate areas. (Ø < 200 mm). The paper reports substantial progress which has been achieved for coating systems with large area substrate holders (up to Ø 1050 mm). The stationary light spot of a single wavelength optical monitor is far out of centre of the rotating substrate holder. Intermittent monitoring on a substrate or a witness is applied. This technique enables rapid prototyping with tight specifications and high yields in large area batch coaters. Application results of challenging optical multilayer systems are demonstrating clearly the potential of this powerful monitoring technique. The monitoring capability was investigated for a lot of different layer systems such as dielectric mirrors, anti-reflection coatings, sophisticated edge filters, polarizer coatings, beam splitters and multiple cavity band-pass filters. Strong coincidence of theory with experiment was achieved with PIAD and magnetron sputtering. Reproducibility experiments have clearly shown the benefits of this monitoring technique.
Real-time lateral optical monitoring for the production of complex multilayer stacks
Catherine Grèzes-Besset, Didier Torricini, Frédéric Chazallet
We present a direct optical monitoring system that allows to minimize in-situ shift of parameters during process. In particular, we show how real-time optical monitoring on one or several lateral samples located on the same circumference of final components overcomes the problem of uniformity time dependence for long process and allows the fabrication of complex optical functions. Real-time signal processing on transmittance versus wavelength is used to determine in-situ refractive index of deposited material for each layer in the multilayer stack. It is shown how this method can be applied to the realization of quarter-wave and non quarter-wave stacks and the repeatability of a fully automated process is demonstrated for different components such as narrow band filters, polarizers or edge filters. Numerous experimental results from different deposition techniques are presented.
Re-engineering of inhomogeneous coatings based on in-situ optical broadband monitoring data
S. Wilbrandt, O. Stenzel, D. Gäbler, et al.
Inhomogeneous layers, such as so-called gradient index layers and rugate filters represent new and prospective thin film designs. Manufacturing such systems in practice requires calculation, deposition, monitoring and characterization of optical coatings with a well-defined continuous refractive index profile along an axis that is perpendicular to the film surface. Those coatings may be manufactured in the Leybold Syrus Pro 1100 deposition system by co-evaporation of SiO2 and Nb2O5 as a sequence of several refractive index gradients. During these experiments our in-situ broadband monitoring system was used to measure the transmittance of the growing film directly at the rotating substrate. This additional information on the intermediate stages of the not yet completed film are extremely helpful in reverse engineering tasks, and clearly superior to the extent of information that may be drawn from the spectra of the completed film only. For characterization of these coatings a new model was developed, which significantly reduces the number of parameters. To generate a feasible parameter set, deposition rates for both materials recorded with quartz crystals monitor during deposition were used. This approach achieves a better accordance between in-situ measured transmittance and modelled transmittance than the intended design. During the optimisation process, a local minimization algorithm was used to vary the refractive index profile of the whole coating and film thickness of the intermediate stages. Finally, a significantly improved accuracy of the modelled transmittance was achieved.
Plasma monitoring of the RLVIP-process with a Langmuir probe
The aim of this investigation was to study the characteristics of a reactive-low-voltage-high-current-ion-plating plasma and to correlate the observed plasma data with the properties of films deposited under such conditions. A Langmuir probe system (Smart Probe - Scientific Systems) was inserted into a Balzers BAP 800 ion plating plant above the e-gun evaporation source close to the insulated substrate holder. In this position during RLVIP deposition, plasma potential, floating potential, self-bias voltage, electron temperature, ion current density, and particle number density were measured and calculated, respectively. All measurements were performed in dependence of arc current (20-80A) and oxygen partial pressure (1 - 36 x 10-4mbar). With rising arc current the number of charged particles, the self-bias voltage between plasma and substrates as well as the energy of the condensing and bombarding species were increased. These data explain the increase of density, refractive index and mechanical stress of RLVIP-metal-oxide-layers, like Ta2O5 and Nb2O5, deposited with higher arc currents. An increase of gas pressure decreased the energy of the particles and therefore reduced slightly film density and refractive index. However, it improved chemistry and eliminated unwanted residual optical absorption and also decreased compressive mechanical film stress.
Ion source characterization based on an array of retarding field analyzers
During the last decade the ever increasing demand for both high-quality optical coatings and virtually deterministic deposition processes has led to a large number of ion sources available for deposition purposes. For a successful implementation of an ion source the prime economic objectives process stability and production yield have to be considered. The economic efficiency is strongly dependent on the temporal stability and spatial distribution of the ion current density and ion energy spectrum. Retarding Field Analyzers have demonstrated their potential as a tool for the analysis of ion sources. However, deliberate evaluation of the measurements is required especially at a non-zero angle of incidence occurring during the examination of three dimensional ion emission profiles. The present study discusses the influence of different geometric Faraday-Cup designs on the resulting data as well as erroneous conclusions potentially drawn from measurements. Furthermore first results of the ion current density distribution characteristics of different ion sources, evaluated on the basis of data taken by a multicup array are presented.
DUV/VUV Coatings I
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IBS deposition of dense fluoride coatings for the vacuum ultraviolet free electron laser
St. Günster, B. Görtz, D. Ristau, et al.
Fluoride materials like Magnesium fluoride and Lanthanum fluoride exhibit unique properties for applications in mirror and anti reflecting coatings in the VUV spectral range (120- 230 nm). These large band gap materials provide low absorption and a usable refractive index contrast. Common deposition methods are thermal evaporation and electron beam evaporation. A columnar microcrystalline structure with a significant porosity is observed for such coatings. Furthermore, a high sensitivity for contamination processes resulting in an increasing absorption is often perceived. Investigations of mirror systems exposed to a harsh environment like the storage ring free electron laser at ELETTRA show a rapid degradation in respect to a reduced reflectivity, an increased hydrocarbon contamination, and a formation of colour centres. An improved performance of the fluoride coatings could possibly be expected for films, which do not have the polycrystalline columnar structure. Ion beam sputtering deposition of fluoride materials demonstrated its applicability to deposit dense amorphous fluoride coatings down to 193 nm. An IBS deposition plant with a Kaufman ion source, using a reactive fluorine environment, is used to grow fluoride layers with comparably low absorption values. Single and multilayer coatings were optically characterised after deposition, exposed to synchrotron radiation at ELETTRA, and characterized again after irradiation. However, the first set of irradiated multilayer mirrors showed a strong degradation of reflectivity and a strong hydrocarbon contamination. Colour centres were not observed.
Performance data of a variable transmission phase shifting mask blank for 193nm lithography enhanced by inspection contrast tuning
Hans Becker, Markus Renno, Ulrich Hermanns, et al.
Schott's already commercially available two layer Ta/SiO2 phase shift system can be tuned from 6% up to 40% transmission for 157, 193 and 248 nm lithography wavelengths. Thus one film patterning process provides a wide product range. Attenuated phase shift masks for 6%, 20% and 30% transmission at 193nm were produced. Tests for laser stability and chemical durability show excellent performance. The phase shifting film achieves a high etch selectivity to the substrate. Dry etch process development is done at IMS chips in Stuttgart, Germany, to provide our customers the service of a good start process for patterning. Results of phase and transmission uniformity are included. Our newest development enhances the layer system and provides a better contrast for inspection in reflection mode. Transmission of our standard two layer Ta/SiO2 PSM system is below the required 20% at inspection wavelengths. The reflectivity of 30% to 40% can be lowered by insertion of an additional contrast layer. The thickness of this contrast layer is adjusted to achieve the required reflection at inspection wavelengths, while the other film thicknesses are tuned to preserve the desired transmission and 180° phase shift at the design wavelength. As first examples 6% and 20% transmission PSM for 193 nm were tested. Reflection at 257 nm and 365 nm inspection wavelengths can be lowered from initial 30% to 40% down to about 10%.
Influence of the amorphous character of Al2O3 layers on their use in the deep UV spectral range
Amorphous layers of metal oxides deposited by Plasma Ion Assisted Deposition (PIAD) are widely used in the field of optical coatings due to their salient properties which enable the deposition of complex multilayer stacks. However, their use in the Deep UV spectral range is restricted as the range of transparency is limited by the absorption due to the first electronic band transition. The only oxide suitable for applications at 193 nm seems to be Al2O3 for which a band gap energy of 8.7 eV (143 nm) is reported for the crystalline state. Yet for thin layers of Al2O3 no work reports the making of absorption free layers at 193 nm. In this study we investigate how the amorphous structure of PIAD-deposited Al2O3 thin films influences the electronic structure and as a consequence of that the absorption behaviour for wavelengths close to the absorption edge. The electronic structure is worked out by a theoretical approach where in a first step the geometric structure is simulated using a Monte Carlo approach. Using this geometric structure the electronic structure is calculated by the tight-binding method in a second step. With these data absorption spectra are calculated and compared to measurements on PIAD Al2O3 layers. The experimental data for the start of the absorption lie on the longer wavelength side of the limit set by the amorphous structure - a fact, that encourages further work on the optimization of the deposition parameters.
Oxide and fluoride coatings for the excimer wavelength 193nm
The requirements to produce high performance coatings increase dramatically when moving from 248 nm to 193 nm. The quality of DUV thin film components is mainly determined by the optical properties of the applied layer materials. The reduction of losses due to scattering and absorption of dielectric materials is essential for excellent properties of the coating results. The most common oxide and fluoride materials SiO2, Al2O3, MgF2 and LaF3 have been investigated and optimized. Plasma ion assisted deposition was applied for the deposition of the oxide materials, using improved coating equipment such as the modified APSpro (advanced plasma source). The paper reports the results of DUV coatings using plasma ion assisted deposition for the oxide materials. Single layers of silica and alumina and multilayer systems with both materials were investigated. In addition, MgF2 and LaF3, conventionally coated at very high temperatures, have been performed to demonstrate the improved capabilities of the optimized SYRUSpro DUV for DUV applications with all the new features.
Aluminum-enhanced optical coatings for the VUV spectral range
This paper deals with the approaches to preserve the high reflectance aluminum mirror for the VUV spectral region. Single fluoride and oxides layer, homogeneous multilayer and hybrid multilayer solutions are put forward. Single fluoride and oxides materials have achieved reflectance above 90% at 193 nm.
DUV/VUV Coatings II
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Lanthanide tri-fluorides: a survey of the optical, mechanical and structural properties of thin films with emphasis of their use in the DUV– VUV–spectral range
H. Uhlig, R. Thielsch, J. Heber, et al.
The present candidates for low loss dielectric optical coatings at VUV excimer laser wavelengths are fluorides. Within this group, only one material - namely lanthanum fluoride - is used almost exclusively as high index film material. In search of additional high index film materials for use in VUV we investigated a broader spectrum of lanthanide tri-fluorides since little is known about their properties and the advantages or disadvantages with regards of their use in DUV- and VUV - optical stacks. Fluorides of lanthanum, neodymium, samarium, gadolinium, ytterbium and also yttrium were evaporated thermally. Precision VUV-measurement were initiated to give an overview of the ranges of UV-transparency up to the absorption edges and to determine the optical indices of these coating materials. Supplementary, also stress measurements, atomic force microscopy and XRD measurements were performed to scrutinize the properties of the films.
Optical, structural, and mechanical properties of gadolinium tri-fluoride thin films grown on amorphous substrates
Roland Thielsch, Joerg Heber, Hein Uhlig, et al.
Since excimer laser applications extend to deep and vacuum UV wavelengths at 248 nm, 193 nm and 157 nm, renewed research interest has recently arisen on fluoride thin films due to their unrivaled position as wide-band-gap material for the vacuum UV (VUV). Among these materials, only a very limited number can act as the high refractive index component in multiplayer interference stacks. Besides LaF3, gadolinium tri-fluoride is a potential candidate especially for wavelengths at about and below 200nm. We report on the evaluation of the structural properties, the optical properties with emphasis to the DUV - spectral range, and the mechanical properties of GdF3 single layer by means of XRD, GIXR, AFM measurements, spectral photometry and by ex - situ mechanical stress analysis using the laser beam deflection method to measure the substrate deformation. The samples were deposited onto fused silica and silicon substrates by a low-loss evaporation technology in a BAK 640 coating plant applying various deposition conditions.
Absorption and fluorescence measurements of DUV/VUV coatings
The performance of optical coatings for high power DUV/VUV laser applications depends amongst others on residual absorption in the thin film layers due to impurities or defects. Using pulsed F2 laser induced fluorescence measurements (LIF), characteristic non-intrinsic emissions of praseodymium, cerium and hydrocarbons are identified for several high reflecting AlF3/LaF3 based mirrors on CaF2 substrates. The separate investigations of single AlF3 and LaF3 layers on silicon wafers indicate that these emissions result from the LaF3 material. The amount of the impurities, however, varies strongly between different LaF3 material grades. The influence of different LaF3 material grades on the absorption properties of high reflecting mirrors is measured for the first time upon ArF laser irradiation using the laser induced deflection technique (LID). Low absorption values of less than 1*10-3 are obtained for all samples. The absorption, however, varies by more than a factor of 2 which is correlated to the appearance of the praseodymium and cerium emissions in the LIF spectra.
Nanostructure and optical properties of fluoride films for high-quality DUV/VUV optical components
Sven Schröder, Hein Uhlig, Angela Duparré, et al.
The persistent utilization of optical lithography at the DUV and VUV excimer laser wavelengths leads to extraordinary demands on the optical components involved (high throughput, low scattering, high mechanical stability, ...). Fluorides are the main or even the only candidates for film materials in these spectral regions because of their low absorption. There are several high-index and low-index fluoride materials. These materials, however, may significantly differ in their nanostructural properties leading to scatter losses crucially influencing the performance of the multilayers. In order to find optimal material combinations, HR multilayer mirrors were fabricated using several high-index fluoride film materials. Spectral photometry, atomic force microscopy, as well as total and angle resolved light scattering measurement and analysis were performed for comprehensive characterization.
XUV Coatings
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Multilayers for the EUV and soft X-ray region
To develop beam splitters for soft X-ray laser Mach-Zehder and Michelson interferometer at 13.9 nm, Mo/Si multilayers deposited on back side and both sides of silicon nitride with thickness of 100 nm were fabricated using DC magnetron sputtering. We presented the results of their reflectivity, transmission and probing the electron density of laser-produced plasma using a soft X-ray laser Mach-Zehder interferometer. The design and fabrication of broadband polarizers were also presented in this paper. These polarizers can be used as analyzers for a wideband polarization measurement. We discuss the results obtained with depth-graded Mo/Si multilayer analyzers for 13-19nm polarization measurements. We also discussed the development of X-ray supermirrors used as broadband angular reflectors operating at the fixed energy of 8 keV. We summarized our recent investigation of the design, fabrication and performance of depth-graded W/Si, W/C and W/B4C multilayers.
Interface-engineered multilayer mirrors
Most applications of Mo/Si multilayer optics in EUVL require a high normal incidence reflectivity. Using dc magnetron sputtering we achieved R = 68.8 % @ λ = 13.5 nm. Different interface-engineered Mo/X/Si/X multilayers with maximum reflectivity of 69.6 % at 13.5 nm were developed. These new multilayer mirrors consist of molybdenum and sili-con layers separated by different interdiffusion barriers (X = C and SiC). Microstructure and optical properties of the multilayers have been investigated by small and large angle Cu-Kα scattering, AFM and characterized by EUV reflectometry. A concept for material selection, thickness optimization of interdiffusion barriers and perspectives for their wide application in imaging EUVL optics will be discussed. Some applications of multilayer mirrors in EUVL require not only the highest possible normal incidence reflectivity but also a long-term and thermal stability at the operating temperatures. The Mo/C/Si/C interface-engineered were optimized in terms of high peak reflectivity at a wavelength near 13.5 nm (Rp ⩾ 60.0 %) and broad operating temperature range (T = 20 - 500°C). The best results were obtained with 0.8 nm thickness of carbon interlayers on both interfaces. Annealing in vacuum was carried out at elevated temperatures up to 650 °C for up to 100 hours. The combination of good optical properties and high thermal stability of interface - engineered Mo/C/Si/C multilayer mirrors underlines their potential for their use in EUVL optics.
X-UV chirped mirror fabrication for phase control of attosecond pulses
In the race towards attosecond (as) pulses for which high order harmonics generated in rare gases are the best candidates, both the Harmonic spectral range and spectral phase have to be controlled. We present in this proceeding four mirrors numerically optimized and designed to compensate for the intrinsic Harmonic chirp recently discovered and which is responsible for a temporal broadening of the pulses. They are capable of compressing the duration down to 100 as. We present the fabrication of those aperiodic multilayers and show the measurement of reflectivity, which prooves that those multilayers are in agreement with the specifications and so let us think that they will be able to compress attosecond high harmonics trains.
Performances and stability of Sc/Si multilayers with barrier layers for wavelengths around 46 nm
Julien Gautier, Franck Delmotte, Marc Roulliay, et al.
We present an experimental study of aging and thermal stability of Sc/Si multilayers deposited by magnetron sputtering. These multilayers have been characterized by using hard X-ray grazing incidence reflectometry at 0.154 nm and synchrotron radiation reflectometry at near normal incidence. The reflectivity was found to be stable after one year. A maximum reflectivity of 46% has been measured at 46 nm. However a 20% relative decrease of the reflectivity have been observed after one hour thermal annealing at 200°C. In order to improve thermal stability, we studied two different barriers layers (B4C and ScN ). We compare the decrease of peak reflectivity and its wavelength shift after one hour annealing at 200°C under argon atmosphere. The best result was observed with the design using 0.3 nm B4C barrier layers. A relative decrease of 2% of the reflectivity peak has been observed with this design as compared to a 20% decrease without barrier layers.
Radiation Resistant Coatings
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Engineering meter-scale laser resistant coatings for the near IR
Laser resistant coatings are needed for beam steering (mirrors), pulse switching (polarizers), and high transport efficiency on environmental barriers (windows / lenses) on large laser systems. A range of defects limit the exposure fluence of these coatings. By understanding the origin and damage mechanisms for these defects, the deposition process can be optimized to realize coatings with greater laser resistance. Electric field modeling can provide insight into which defects are most problematic. Laser damage growth studies are useful for determining a functional laser damage criteria. Mitigation techniques such as micro-machining with a single-crystal diamond cutting tool or short pulse laser ablation using the burst technique can be used to arrest growth in damage sites to extend optic lifetime.
Comparative study of IR and UV laser damage resistance of silica thin films deposited by Electron Beam deposition, Ion Plating, Ion Assisted Deposition and Dual Ion Beam Sputtering
The laser damage resistance of optical coatings is a critical point for a large number of applications. However improving this resistance is often hard to obtain because of the large number of parameters in the deposition processes than can modify the laser damage threshold and the lack of detailed and exploitable studies published on this subject. Then, the aim of this work is to test and analyze the laser damage resistance of a usual material for high power applications (silica) deposited in various conditions. The thin films of different thicknesses were specially deposited using different techniques available at the Institut Fresnel: Dual Ion Beam Sputtering, Electron Beam Deposition, Ion Assisted Deposition and Ion Plating. The laser-induced damage thresholds of these coatings were determined at 1064nm and 355nm using nanosecond pulsed YAG lasers, with a 1-on-1 test procedure. Other diagnostic tools were used to complete the study and make potential correlations with laser damage: photothermal techniques, luminescence spectrocopy, optical profilometry, dark field and Nomarski microscopy. The comparative study of these results highlight different laser damage behaviors of the silica coatings that we correlate to the density and the nature of the defects.
LIDT improvement of multilayer coatings by accurate analysis of fabrication steps
We present Laser Induced Damage Threshold (LIDT) results on multilayer components with different optical functions for near infrared applications. In this paper, we investigate the different fabrication steps of such functions. In particular, we show experimental results on surface preparation (polishing, cleaning,) and on deposition techniques (Ion beam assisted process) related to the materials involved in coatings. Laser damage tests are performed at 1064-nm with a 5-ns pulse Nd:Yag laser and experiments are made at surfaces of optical components using a 12 μm diameter focused beam. Accurate damage probability curves are plotted thanks to a reliable statistical measurement of laser damage. Use of a statistical model permits to deduce the densities of laser damage precursors. A systematic analysis of all the steps involved in fabrication allows then to build multilayer components with high laser induced damage resistance.
Laser thin films with very high damage threshold
Jianda Shao, Zhengxiu Fan
New developments of laser thin films for high power laser systems were reviewed. Special attention was paid to several key coatings which bottlenecked the higher power laser system, such as pick-off mirrors, large aperture polarizer and YAG harmonic wavelength splitter, as well as AR coatings. Defects were deemed to be the initial and essential source of laser-induced damage. The investigation of the original control of defects was focused on the deposition process control, such as substrate cleaning, purity of deposition materials, deposition temperature, oxygen pressure in vacuum chamber and so on. Several methods of evaluation of laser damage were employed, which included Laser Induced Damage Threshold (LIDT) determination and absorption detection based on Surface Thermal Lensing (STL) technique, as well as Total Integrated Scattering (TIS) measurement. The LIDT of pick-off mirrors reached to 20 J/cm2 (1064 nm, 1 ns), meanwhile the LIDT of the ultraviolet coatings did to 8 J/cm2 (355 nm, 1 ns) because of its comprehensive mechanism. The LIDT of third harmonic mirror could be improved effectively with post-treatment methods, such as oxygen-plasma post-treatment and vacuum annealing. Actually the situation of the laser thin films with very high damage threshold was complicated due to their uniformity of optical properties and stress induced surface deformation in the large aperture.
Manufacturing I
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Ion beam sputter coatings for laser technology
Detlev Ristau, Tobias Gross
The initial motivation for the development of Ion Beam Sputtering (IBS) processes was the need for optical coatings with extremely low optical scatter losses for laser gyros. Especially, backscattering of the gyro-mirrors couples the directional modes in the ring resonator leading to the lock in effect which limits the sensitivity of the gyro. Accordingly, the first patent on IBS was approved for an aircraft company (Litton) in 1978. In the course of the rapid development of the IBS-concept during the last two decades, an extremely high optical quality could be achieved for laser coatings in the VIS- and NIR-spectral region. For example, high reflecting coatings with total optical losses below 1 ppm were demonstrated for specific precision measurement applications with the Nd:YAG-laser operating at 1.064 μm. Even though the high quality level of IBS-coatings had been confirmed in many applications, the process has not found its way into the production environment of most optical companies. Major restrictions are the relatively low rate of the deposition process and the poor lateral homogeneity of the coatings, which are related to the output characteristics of the currently available ion sources. In the present contribution, the basic principles of IBS will be discussed in the context of the demands of modern laser technology. Besides selected examples for special applications of IBS, aspects will be presented for approaches towards rapid manufacturing of coatings and the production of rugate filters on the basis of IBS-techniques.
Highly reflective thin film coatings for high power applications of micro scanning mirrors in the NIR-VIS-UV spectral region
This paper addresses different highly reflective optical coatings on micro scanning mirrors (MSM) for applications in the NIR-VIS-UV-spectral region to enable new applications at high optical power density like laser marking and material treatment. In the common case of MSM with an unprotected Al coating, the absorption limits the maximal power density because of induced heating. In contrast to macroscopic optics HR-micro mirror coatings have to guarantee additional demands like low-stress and CMOS compatibility. Hence, to enable novel high power applications of MSM in the NIR-VIS-UV spectral region highly reflective low-stress coatings have been developed according to a triple strategy: (a) broadband metallic reflectors, (b) dielectric multilayers and (c) enhanced hybrid coatings. For Au and Ag based NIR-coatings an excellent mirror planarity and a reflectance around 99 % (@ 1064 nm) have been achieved, whereas dielectric coatings reached 99.7 % for a (LH)4 design and thinner low-stress hybrid NIR-coatings reached up to 99.8% enabling an improved mirror planarity and excellent laser damage threshold. For the VIS and UV spectral region enhanced hybrid HR-coatings have been favored, because they enable high reflectance of up to 99.7 % @ 633 nm or 98.8 % @ 308 nm in combination with low stress, high mirror planarity and CMOS compatibility.
Temperature dependence of the optical properties of mixed oxide thin films deposited by reactive magnetron sputtering
M. Vergöhl, B. Hunsche, A. Ritz
The optical properties of TaZrOx mixed oxide thin films are investigated. The films were deposited by reactive pulsed magnetron sputtering in a double magnetron set up using two Ta and Zr metallic targets. Depending on the mixture of the materials, crystallization at different temperature occurs. For a specific mixture, temperature stability of more than 950°C could be demonstrated. This is more than another value of TiAlOx thin films reported very recently.
Manufacturing II
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Correlation between the optical performance of TiO2-Ag-TiO2 multilayers and the interface roughness between the layers
Ag-dielectric multilayers are widely used in the production of heat reflecting filters, induced transmission filters, beam splitters, etc. The performance of such coatings in the visible part of the spectrum is sometimes strongly influenced by a plasmon absorption in the Ag-layer or a surface plasmon absorption in the Ag-dielectric interfaces. The strength of the plasmon absorption is very sensitive to the layer structure, the light polarization and the angle of incidence. As a result, the target specifications for reflection and transmission are not reached easily. We investigate PVD-deposited TiO2-Ag-TiO2 multilayers by means of optical reflection and transmission and Grazing Incidence X-ray Reflectometry (GIXR). The GIXR-method yields the individual layers thicknesses and the interface roughness. Some of the coatings have a broad absorption peak between 500 and 400nm that cannot be modeled using the bulk dielectric function of Ag. The magnitude of the absorption peak is correlated with the measured roughness of the TiO2-Ag interfaces. The analysis of the results shows the critical parameters for the deposition process.
High-rate deposition of optical coatings by closed-field magnetron sputtering
D. R. Gibson, I. Brinkley, E. M. Waddell, et al.
"Closed field" magnetron (CFM) sputtering offers a flexible and high throughput deposition process for optical coatings and thin films required in a wide range of optical applications. CFM sputtering uses two or more different metal targets to deposit multilayers comprising a wide range of dielectrics, metals and conductive oxides. Moreover, CFM provides a room temperature deposition process with high ion current density, low bias voltage and reactive oxidation in the entire volume around the rotating substrate drum carrier, thereby producing films over a large surface area at high deposition rate with excellent and reproducible optical properties. Machines based on the Closed Field are scaleable to meet a range of batch and in-line size requirements. Typically, thin film thickness control to <±1% is accomplished simply using time. Fine layer thickness control and deposition of graded index layers is also assisted with a specially designed rotating shutter mechanism. The CFM configuration also allows plasma treatment of surfaces prior to deposition, allowing optimisation of coating adhesion to substrates such as plastics. This paper presents data on optical, durability and environmental properties for CFM deposited optical coatings, including anti-reflection, IR blocker and colour control and thermal control filters, graded coatings, as well as conductive transparent oxides such as indium tin oxide. Benefits of the CFM sputter process for a range of optical applications are described.
Innovative production of thin film laser components
Michael Scherer, Harro Hagedorn, Walter Lehnert, et al.
Future production of high quality laser components asks for both, the precise preparation of low loss multilayer stacks and a clean room compatible innovative deposition process. In addition a cost-effective thin film filter production is required in order to transfer new developments like ultra fast pulse laser technique from research to economical products and applications. One of the most promising candidates is magnetron sputtering due to the potential of excellent film properties, a fully automatic clean room compatible manufacturing process and a high productivity. Similar film qualities as with ion beam sputtering are realised but with a more than 10 times higher productivity. The reproducible production of multilayer broad band mirrors with controlled group delay dispersion and low losses is still a big challenge. Promising results were achieved on the basis of silica and niobia and will be presented.
Thorium-free interference coatings for infrared applications
Sven Laux, Helmut Bernitzki, Dieter Fasold, et al.
This paper discusses improvements in manufacturing of coated infrared optical components. Such components often have key functions in defence, security or space applications and must withstand severe environmental conditions. Therefore, very durable coatings are desired. As a consequence of its radioactivity the formerly used low refractive index material thorium fluoride is substituted. Examples for beam splitter cubes contacted with novel infrared transparent cement, interference filters, mirrors and AR coatings are presented.
Precision optical and antireflection multilayer and gradient coatings containing reactively sputtered oxides, nitrides and fluorides
H. Bartzsch, P. Frach, J. Weber, et al.
Optical coatings have been deposited by pulse magnetron sputtering of the target materials silicon and aluminium using the reactive gases oxygen, nitrogen and fluorine. The measured refractive index and roughness of the SiO2, Si3N4, Ta2O5 and Al2O3 films indicate the deposition of very dense and smooth films. Absorption of SiO2 and Al2O3 films is low even at a wavelength of 193nm. The sputter deposited AlF3 layers have low absorption until 150 nm but then show an absorption edge. Examples of multilayer include antireflective coatings for ophthalmic lenses and cut filters consisting of up to 150 λ/4 layers. These films were produced at a single stationary coating station without interruption of film deposition by changing the reactive gas during the plasma process. This process was also used for the deposition of rugate filters with apodisation function by continuous variation of the reactive gas composition during the deposition.
Manufacturing III
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Organically modified SiO2 coatings on polycarbonate
Improvements of the environmental stability of inorganic optical coatings on polymer substrates are expected from a slight variation of the chemical composition of SiO2 films by organic modification through the addition of gaseous hexamethyldisiloxane (HMDSO) to a classical plasma ion-assisted deposition process. The influence of several process parameters on the chemical composition of these coatings has been studied on polycarbonate, quartz glass and silicon substrates to define an optimum range of process parameters with regard to the useful properties obtained of the coated polymer optical component.
Design of hybrid coatings composed of homogeneous layers and refractive index gradients
Inhomogeneous coatings are promising for superior optical properties, e.g. broadband antireflection, in comparison to conventional HL-stack designs. Although a lot of excellent theoretical work on optical behaviour of rugates and gradient index films has been done during the last decades, there is no real breakthrough in industrial fabrication. The realization of such coatings leads to an extensive and time-consuming computer-aided control, because of complicated layer designs with continuously changing refractive index gradients. We describe the design and optical performance of an omnidirectional antireflection coating that essentially represents a hybrid coating composed from homogeneous layers and linear refractive index gradient layers.
Gravure printing of transparent conducting ITO coatings for display applications
Joerg Puetz, Sabine Heusing, Marcos de Haro Moro, et al.
Transparent conducting coatings and patterns of ITO (indium tin oxide) were deposited by a direct gravure printing on PET foils using nanoparticle-based UV-curable inks. Solid areas with thicknesses ranging between 300 and >1000 nm were obtained by varying the ink composition (e.g. ITO content, solvents) and fundamental parameters of the printing plate such as the line density. The best ITO coating patterns showed a sheet resistance of 3 to 10 kΩ and a transmission of up to 88 % with a haze of less than 1 %. One of the most crucial steps during film formation is the drying of the wet film as it changes the rheology and polarity of the ink and in consequence decisively influences the film formation. Typical fields of application of the gravure-printed ITO patterned electrodes include smart windows, flexible displays and printed electronics.
Optical and mechanical properties of thin RLVIP Nb2O5-films
Thin Nb2O5-films were deposited on unheated glass, fused silica, and silicon substrates by reactive-low-voltage-high-current-ion-plating (RLVIP). Optical as well as mechanical film properties and their environmental stability are remarkably influenced by deposition parameters like e. g. arc current, deposition rate, gas composition, and total gas pressure. It was found out that an arc current around 50A, gas mixtures with high amount of oxygen, and a deposition rate around 0,3nm/s yielded the best results. Refractive indices were calculated from data obtained by spectrophotometric intensity measurements of the constrained amorphous and homogeneous films. Residual optical absorption in the film's high transmittance range was determined by photothermal deflection spectrometry. Mechanical film stress, for dense films always compressive, was measured by deformation of coated thin silicon discs. Typical obtained values are n550 = 2,39 - 2,40, k515 = 2×10-4, σ = -30MPa. Detailed information is presented in diagrams.
Chemical vapour deposition of optical coatings onto small scale complex optical components
M. L. Hitchman, D. R. Gibson, W. Manookian, et al.
In this paper we describe how optical coatings can be deposited uniformly with a high precision and reproducibility on 3-dimensional substrates, such as spherical lenses, by CVD. We present results that will highlight some specific advantages of CVD over the traditionally used methods of e-beam evaporation and magnetron sputtering and we will show that CVD has tremendous potential for enhancing the quality of optical coatings and for making cost savings.
Poster Session
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Comparison of optical resistance of ion assisted deposition and standard electron beam deposition methods for high reflectance dielectric coatings
A. Melninkaitis, M. Maciulevicius, T. Rakickas, et al.
The ion assisted thin film deposition (IAD) method has been used extensively for more than two decades, but questions about possibility of improving of the laser-induced damage threshold (LIDT) by this method compared with the conventional electron-beam evaporation (non-IAD) method are still not fully answered. A more complete understanding of different factors that can influence laser-induced damage threshold is necessary for continued development of multilayer dielectric coatings optimized for high-power laser applications. To clarify these factors we performed comparison of LIDT for IAD and non-IAD coatings in nanosecond and femtosecond pulse ranges. High reflectance mirrors at 800 nm and 532 nm were tested. Mirror coatings were made of ZrO2 and SiO2. Automated LIDT measurements were performed according to the requirements of current ISO 11254-2 standard. Two lasers were used for the measurements: Nd:YAG (λ = 532 nm, τ = 5 ns) and Ti:Sapphire (λ = 800 nm, τ = 130 fs). Measurements at 800 nm and 532 nm were performed at 1-kHz and 10 Hz pulse repetition rate respectively (S-on-1 test). The damage morphology of coatings was characterized by Nomarski microscopy and relation of LIDT with coating parameters was analyzed.
Multiple pulse laser-induced damage of antireflection coated lithium triborate
A. Melninkaitis, D. Miksys, R. Grigonis, et al.
An investigation of laser-induced damage thresholds (LIDT) of antireflection coated lithium triborates used for second and third harmonic generation were performed at 1064, 532, and 355 nm wavelengths for ~4 ns pulses. Two types of coatings were tested: an anti-reflection coatings with dual peak at 1064 nm and 532 nm and anti-reflection coatings with three peaks at 1064 nm, 532 nm, and 355 nm, respectively. Ion-beam sputtering and magnetron sputtering technologies where used for coatings deposition. Automated LIDT measurements were performed according to the requirements of current ISO 11254-2 standard. The obtained LIDT were in range of 3-15 J/cm2.
Optical sensitivity of thin films to hydrocarbons and ozone
Thomas Mazingue, Lorenzo Spalluto, Ludovic Escoubas, et al.
Materials involved in gas sensing applications have been deposited by various methods in thin film form. Variation of the optical properties of the thin films were investigated under butane and ozone exposure using the m-lines technique. Effective index variations down to 10-4 were observed. Concentrations of 100 ppm of butane diluted in the air or in nitrogen were detected.
Growth and thermal stability of interfaces in ion beam sputtered Mo/Si mirrors
E. Quesnel, C. Largeron, V. Muffato, et al.
In the field of microelectronics, the Extreme Ultraviolet (EUV) lithography operating at λ=13,5 nm, appears, today, as the most promising future technology. The viability of this next generation technology has, however, to face several technical issues. Among them, the realisation of highly reflective EUV mirrors is one of the key issues and concerns the mirrors for light transport as well as the lithography masks. In this last case, the mirrors which consist in a periodic Mo/Si multi-layer coating deposited by ion beam sputtering suffer from reflectance limitations and thermal instabilities. In this paper, an experimental investigation on IBS deposited Mo/Si multi-layers is presented. The study is mainly focused on the formation of Mo/Si interfacial zones and their evolution with thermal annealing up to 600°C. Detailed investigations by high-resolution transmission electron microscopy (HRTEM) and energy filtering TEM have been performed in association with differential scanning calorimetric (DSC) analyses. For the purpose, dedicated samples were prepared enabling the identification of phase transformations occurring during thermal annealing. It will be shown, in particular, how this coupled characterisation approach (TEM+DSC) can help understanding the interface growth in such metal/silicon systems. The characterisation results are presented and discussed.
Zr–silicate co-evaporated thin films
J. Ciosek, W. Paszkowicz, A. Kudla, et al.
Thin films of Zr-silicate were deposited on silicon and BK7 glass substrates by EB co-evaporation. The mixing thermodynamics of the ZrO2 - SiO2 system was analysed. Chemical bonding in Zr-silicates has been studied by X-ray photoelectron spectroscopy. The structural and optical properties and the surface morphology were investigated.
Properties of chirped mirrors manufactured by plasma ion assisted electron beam evaporation
Martin Bischoff, Olaf Stenzel, Dieter Gäbler, et al.
Nowadays, chirped dielectric mirrors for ultrafast optics and laser applications are usually manufactured by sputtering techniques. The suitability of Advanced Plasma Source (APS) assisted electron beam evaporation with respect to such coatings is still under investigation. The purpose of this presentation is to show our first results of the deposition of chirped layers produced by plasma ion assisted electron beam evaporation and of the investigation of their properties. The aim was to design and prepare a NIR-mirror for the spectral range of 700 nm to 900 nm. It has been attempted to find a design that is robust with respect to errors of thickness and refractive index. The mirror consists of more than 26 layers composed of alternating high- (Nb2O5) and low-refractive index (SiO2) material. The deposited coatings were tested in terms of their group delay dispersion (GDD) and their reflectivity. We show, that in the wavelength range between 720 nm and 890 nm the GDD exhibits a value of about -50 fs2, whereas the reflectivity is above 99%. However, the subsequent reverse engineering operations show a relatively large thickness error of more than 1% - 2% regarding the particular layers. Nevertheless the effect on the GDD and the reflectivity is tolerable. Furthermore, we present our first experiments concerning the design and fabrication of a chirped mirror, which allows controlling the third order dispersion (TOD), whereas the relative thickness error of the particular layers should not exceed 1%.
Comparison of gradient index and classical designs of a narrow band notch filter
Vesna Janicki, Marc Lappschies, Björn Görtz, et al.
Rugate structures, as well as gradient refractive index films in general, attract a lot of interest. The gradient index systems may provide advantages in both, optical performance and mechanical properties of the optical coatings. Rugates have shown to be especially interesting for design of notch filters. A lot of theoretical work on design of rugate filters has been done in the last decades. However, only few of the designs could be deposited, which is often caused by practical problems, e.g. preparing materials with the desired refractive index values. In this paper two different gradient refractive index designs are compared to a classical high-low stack. One gradient design is synthesized by an apodized sinusoidal structure that is approximated by homogeneous sublayers. The other one is based on an apodized sinusoidal structure as well, but it is approximated by a hybrid structure, i.e. a combination of linear gradient index ramps between the lowest and the highest refractive index applicable and homogeneous layers of high index values. The two gradient designs take into account the constraints posed by limitations of the real deposition systems. Both designs are compared to a classical high-low stack and the advantages and drawbacks of each approach are commented.
Synthesis and manufacturing the mirrors for ultrafast optics
Vladimir Pervak, Sergey Naumov, Gabriel Tempea, et al.
Properties of 3 types of multilayer dielectric chirped mirrors manufactured with Helios Leybold system (magnetron sputtering with plasma/ion assisted technology) are discussed. The first type includes mirrors providing negative group delay dispersion (GDD) and high reflectance in a wavelength range 650-1150 nm. Such mirrors are used in a broadband Ti:Sapphire oscillator for generating sub-6 femtosecond pulses. The second type of mirrors has extremely low both GDD oscillations and losses in a range 740-840 nm. Such mirrors are of interest for both long-cavity high-energy Ti:Sapphire oscillators and so-called external cavities for storing energy from femtosecond oscillators. The lowest residual GDD fluctuations achieved for this type of mirrors are 5 fs2. The third type is high reflectors with very high reflectivity. Different coating materials: Nb2O5, TiO2, Ta2O5 together with SiO2 are compared for these 2 types of mirrors. The results of reproducibility of such mirrors and their characterization in terms of reflectivity, losses, surface quality are presented. Comparison of the design with the manufactured mirror is also done.
Optical thin films deposition by MDECR-PECVD
Bicher Haj Ibrahim, Pavel Bulkin, Dmitri Daineka, et al.
We designed and built Matrix Distributed ECR (MDECR) PECVD reactor dedicated for dielectric filters deposition and equipped it with multiple sensors for process control. Planar matrix geometry of plasma source is based on electron cyclotron resonance effect at 2.45 GHz microwave frequency and provides scalability of the deposition on large area substrates. High (up to 5 nm/sec) deposition rate obtained due to high dissociation efficiency and careful design of the gas injection system. Optical emission spectroscopy, quadrupole mass-spectrometry and spectroscopic and multi-channel kinetic ellipsometry are installed for in-situ studies and control of the film deposition. We performed studies of the nature of high-density plasma discharge in silane, oxygen and nitrogen mixture and correlated its properties with optical and physical properties of deposited materials. To demonstrate the capabilities, a wide band gradient index antireflection coating on glass was realized by deposition of SiOxNy alloy thin films. The predefined variation of an index in a profile is obtained by changing the flows of precursors. Real-time control is performed with multi-channel kinetic ellipsometry.
Ageing of optical components under laser irradiation at 532nm
S. Becker, L. Delrive, P. Bouchut, et al.
The pulsed Laser Induced Damage Threshold (LIDT) of optical components usually reaches several hundreds of MW/cm2. When exposed to laser power several order of magnitude below their LIDT, the optical component lifetime is, by default, considered infinite. Under specific conditions, the accumulation of laser pulses may lead to a contamination of the surface and a degradation of its optical properties and LIDT. In the first order, these phenomena depend on the experimental conditions such as the irradiation time, the laser power, and the environment. In order to better understand the physics emphasizing this degradation, we developed an experimental cell with an in-situ spectroscopic ellipsometry diagnostic. The dry-pumped cell sheltering the sample is associated with a mass spectrometer that enables us to follow the environmental conditions in which we experiment the ageing. Anti-reflection coatings on fused silica were tested under 10 kHz-532 nm laser ageing. We present first results of degradation obtained in these conditions.
Determination of complex optical indices in the 80-140nm VUV wavelength region from reflectivity measurements under normal incidence: application to ZnSe
F. Bridou, M. Cuniot-Ponsard, J. M. Desvignes
The observation of hot plasmas in the interstellar medium requires efficient mirrors in the 80-120 nm wavelength range. Contrary to that of most metals, the high reflectivity of pure aluminum is maintained close to 80% in this range. Unfortunately, it is drastically reduced to values lower than 10% by the strongly absorbing thin alumina layer which spontaneously forms upon air contact. We report here the results obtained with a capper layer of ZnSe. The optical indices given for this material by Palik's tables lead to predict a resulting high reflectivity, provided the layer prevents oxidization of underlying Al. The measured reflectivity does not agree with theory. The reasons for this inconsistency are examined. It is shown that complex indices of ZnSe in the wavelength region between 80 and 140 nm can be extracted. from the reflectivity measurements obtained with different ZnSe thicknesses on Al. The imaginary part of the index is then found to differ strongly from Palik's tables value.
High-performance Cr/Sc multilayers for the soft x-ray range
Results of soft x-ray reflection measurements of Cr/Sc multilayer mirrors close to the Sc-L (λ = 3.11 nm) and C-K (λ = 4.44 nm) absorption edges are presented. In particular, normal-incidence reflectivity measurements performed at BESSY II facility revealed a reflectivity of R = 17.3% @ 3.11 nm and 7.0 % @ 4.44 nm. Simulation results show that the interface roughness in the best Cr/Sc structures are less than 0.4 nm and strongly depend on the crystal-line structure of the layers.
Ion-assisted deposition of SiO2 film from silicon
Tuan.H. Pham, Cu. X. Dang
Silicon dioxide, SiO2, is one of the preferred low index materials for optical thin film technology. It is often deposited by electron beam evaporation source with less porosity and scattering, relatively durable and can have a good laser damage threshold. Beside these advantages the deposition of critical optical thin film stacks with silicon dioxide from an E-gun was severely limited by the stability of the evaporation pattern or angular distribution of the material. The even surface of SiO2 granules in crucible will tend to develop into groove and become deeper with the evaporation process. As the results, angular distribution of the evaporation vapor changes in non-predicted manner. This report presents our experiments to apply Ion Assisted Deposition process to evaporate silicon in a molten liquid form. By choosing appropriate process parameters we can get SiO2 film with good and stable property.
B4C/Mo/Si multilayers for 20–40 nm wavelengths: application to broadband mirrors
Franck Delmotte, Julien Gautier, Marc Roulliay, et al.
Theoretically, periodic three component multilayers as B4C/Mo/Si allow an improvement of the reflectivity in the 25 nm-40 nm range as compared to two component multilayers as B4C/Si. Optimized B4C/Mo/Si and B4C/Si multilayers have been deposited by magnetron sputtering and ion beam sputtering. The multilayers have been characterized by x-ray grazing reflectometry (λ = 0.154 nm) and synchrotron radiation measurements at near normal incidence. The maximum experimental reflectivity for B4C/Si is 25% at 32 nm and 23% at 38 nm. For B4C/Mo/Si multilayers, we obtained an experimental reflectivity of 34% at 32 nm and 29% at 39.5 nm. Moreover the width of the Bragg peak is larger for B4C/Mo/Si than for B4C/Si. We have used these multilayers in a non periodical structure in order to produce broadband mirrors. It consists of the superposition of two periodic B4C/Mo/Si multilayers with different period thickness. Theoretical optimization of such structure by simulation is presented. Preliminary experimental results demonstrate the interest of such structure : two broadband mirrors have been deposited and measured over a wide wavelength range (12 nm to 45 nm). The first mirror presents a broadband spectrum centered at 32 nm with peak reflectivity of 22% and bandwidth larger than 9 nm. The second mirror has been optimized to produce theoretically an average reflectivity of 19% from 25 nm to 35 nm.
Optical monitoring of rugate filters
Marc Lappschies, Björn Görtz, Detlev Ristau
Rugate filters have a high potential for solving specific design problems in many applications of modern optics and lighting technology. However, the exact manufacture of these gradual layer systems is still a challenge which could not be solved completely until today. One of the prominent approaches for the production of rugate filters is based on independent quartz crystal devices measuring the rate of the different coating materials. As an alternative, optical broadband monitoring has been already qualified for controlling the deposition of complicated non quarterwave stacks. In the present study, promising results of this deposition control concept as a direct monitoring of rugate filters will be presented. In a first attempt, the continuous change of refractive indices in the graded layers was transformed to a set of discrete homogeneous sub-layers with thicknesses values of around 5 nm. These discrete layers are realized by defined mixtures of two materials. A data base for the dispersion behavior was created for the different mixing ratios and is employed for the production of such quasi-rugate filters. The optical monitor is operated in the routine mode determining the switching points of the layers. Selected examples will be presented for quasi rugate coatings produced by ion beam sputtering from a movable zone target. Different designs will be discussed considering production problems as well as achievable optical properties.
Effective medium models for metal-dielectric composites: an analysis based on the spectral density theory
We study different effective medium theories for describing the optical behaviour of composites consisting of spherical metallic inclusions embedded in a dielectric matrix. The analysis is performed according to the Bergman spectral density theory. This theory establishes that any effective medium model has an integral representation in terms of a function (the spectral density) that depends on the geometry of the two-phase mixture and is independent of the optical constants of the composing materials. We review classical effective medium theories (Maxwell-Garnett and Bruggeman models) according to their spectral density. Furthermore, numerical simulations based in recent works allow studying the influence of different geometric parameters in the spectral density and compare the results with the classical theories.
Design elements of porous silicon omnidirectional mirrors
E. Xifré-Pérez, J. Ferré-Borrull, J. Pallarès, et al.
Omnidirectional mirrors are multilayer periodic structures that reflect light in a wide range of wavelengths for all angles of incidence and for all polarizations of the incident light. These structures can be made using the porous silicon technology: the layers are electrochemically etched to have different porosities, corresponding to different refractive indices. Since the porosity depends on the current density of the electrochemical etching process, the layers may have any refractive index value from 1.2 to 2.7. In opposition to classical evaporated thin films where the refractive indices are fixed, this offers a new degree of freedom in the design of such structures. In this work, the four main parameters of a basic omnidirectional mirror (refractive index of the two kinds of layers and their optical thicknesses) are analyzed to find the condition to obtain the maximum width of the omnidirectional reflection band. The analysis is made using the framwork of the Photonic Band Gap materials and considering the omnidirectional mirrors as 1-D Photonic Crystals.
VUV optical coatings for the next-generation micro-mechanical mirrors
This paper deals with vacuum UV optical coatings for micro mirrors applications. High reflecting low-stress optical coatings for the next-generation of micro mechanical mirrors have been developed. The optimized metal systems are applicable for the VUV spectral region and can be integrated in the technology of MOEMS, such as spatial light modulators (SLM) and micro scanning mirrors.
High resolution video based inspection method for LIDT investigations of thin disc laser crystals
Past investigations in the damage threshold of laser components have been of high interest within optics characterization. In view of the ever increasing complexity of optical components investigations in the LIDT require a more sophisticated adaptation of the measurement set-ups. The optimization of high power solid state laser systems led to the disc laser concept, which provides an increased output power. The achievable output power is mainly limited by the damage threshold of the coated and bonded crystal. Consequently, the understanding of damage mechanisms is a fundamental requirement for the disc laser optimization. It is assumed that the damage in disc laser crystals and deposited coatings can be traced back to the defects on the crystal surface or in the optical coatings. The expected size of the defects initiating laser damage ranges in the micrometer scale. In the present study, LIDT experiments are focused on the verification of this assumption and are intended to assist in the optimization of the manufacturing process. For a detection of the defects, an online defect inspection system was extended by a highly resolving imaging technique. The LIDT measurements have been performed on the basis of the Son1 protocol according to ISO 11254-2 at an effective pulse duration of about 11ns and a repetition rate of a few Hz at the wavelength 1.064nm.
Laser ablation of SiOx thin films for direct mask writing
J. Heber, J. Ihlemann, M. Schulz-Ruhtenberg, et al.
The present study of silica thin films illustrates a new way of direct writing diffractive phase elements by means of UV laser ablation. The concept consists in the conversion of highly absorbing silica layers, which are suitable for laser ablation, into UV transparent structures by thermal annealing, after a direct laser patterning process. This concept has been investigated in detail for several process parameters. As example, a pixel pattern, generated by an appropriate optical design algorithm, is transferred into a phase delay pattern in form of a silica surface relief, which results in a diffractive shaping of a beam transmitted (or reflected) by this structured layer. The direct mask patterning could be achieved at a moderate laser fluence of 350 mJ/cm2 with a 248 nm excimer laser.
Deposition of broadband antireflection coatings on plastic substrates by evaporation and reactive pulse magnetron sputtering
Evaporation and reactive pulse magnetron sputtering are two methods to deposit broadband antireflection coatings at low temperatures. The performance of broadband antireflective coatings on polycarbonate (PC) deposited by these methods is shown. Plasma-treatment of the plastic substrates has an important effect on the adhesion of the coating system on the substrate. For sputtering different parameter sets for the pre-treatment as well as the deposition pressure and their effect on adhesion were examined for polycarbonate substrates. Furthermore evaporation and reactive pulse magnetron sputtering were compared with regard to the adhesion of broadband antireflective coatings on PC.
New advances in improving low-temperature stability of infrared thin-film interference filters
B. Li, S. Y. Zhang, D. Q. Liu, et al.
The degeneration of performance of an optical thin-film interference filter associated with the change of temperature is not acceptable. In this letter, we report a new progress in improving low-temperature performance of infrared narrow-band filters by using Pb1-xGexTe initial bulk alloy with appropriate Ge concentration x. It can be found that there exists a critical temperature for the investigated narrow-band filter, at which the temperature coefficient of filter is exactly zero. Therefore, by means of controlling the composition in (Pb1-xGex)1-yTey layers, the temperature coefficient of filter can be tunable at the designated low-temperature. In our present investigation, when temperature varies from 300 to 85 K, a shift of peak wavelength of 0.05935 nm.K-1 has been achieved.
Optical characterization of non-uniform thin films using imaging spectrophotometry
Miloslav Ohlídal, Vladimir Cudek, Ivan Ohlídal, et al.
In this paper the method of imaging spectrophotometry enabling us to characterize non-absorbing thin films non-uniform in the optical parameters is described. This method is based on interpreting the spectral dependences of the local absolute reflectances measured at the normal incidence of light. It is shown how to determine the area distribution of thickness and refractive index of the non-absorbing non-uniform thin films by treating these reflectances. Moreover, the generalization of the method for the optical characterization of slightly absorbing non-uniform thin films is also indicated. Furthermore, the two-channel imaging spectrophotometer enabling us to apply the method of imaging reflectometry is described. The procedure for determining the spectral dependences of the local absolute reflectance in the points aligned in a matrix situated on the illuminated area of the non-uniform thin film by means of the spectrophotometer is also presented. The practical advantages of the method are specified. The method is illustrated by means of the optical characterization of a selected epitaxial ZnSe thin film prepared using molecular beam epitaxy onto gallium arsenide single-crystal substrate.
Deposition of robust multilayer mirror coatings for storage ring FEL lasing at 176nm
St. Günster, D. Ristau, M. Trovó, et al.
Progress was achieved in the last years in the development of multilayer mirrors used in storage ring Free Electron Lasers (FEL) operating in the vacuum ultraviolet spectral range. Based on dense oxide coatings deposited by Ion Beam Sputtering, a stable lasing at 190 nm was demonstrated. The extension towards shorter wavelengths had to overcome severe problems connected to the radiation resistance and the necessary reflectivity of the resonator mirrors. In this context, radiation resistance can be considered as the ability of the mirror materials to withstand the high power laser radiation and the intense energetic background radiation generated in the synchrotron source. The bombardment with high energetic photons leads to irreversible changes and a coloration on the specimen. Reflectivity requirements can be evaluated from the tolerable losses of FEL systems. At ELETTRA FEL the resonator mirror reflectivity must be above 95 %. Evaporated fluoride multilayer mirrors provide sufficient reflectivity, but they do not exhibit an adequate radiation resistance. Pure oxide multilayers show a sufficient radiation resistance, but they cannot reach the necessary reflectivity below 190 nm. A successful approach combines evaporated fluoride multilayer stack with a dense protection layer of silicon dioxide deposited by Ion Beam Sputtering. Such mirror systems were produced reaching a reflectivity of approximately 99 % at 180 nm. Lasing in the storage ring FEL at ELETTRA was realised in the range between 176 - 179 nm. The mirror reflectivity shows only a slight degradation after lasing, which could be fully restored after the lasing experiment.
Spatial beam switching using the superprism effect in nonlinear thin-film stacks
Thin-film stacks exhibiting a high spatial dispersion similar to the photonic crystal superprism effect can be employed to multiplex or demultiplex several wavelength channels using a single thin-film stack. The phase properties of these stacks are designed such that a small change in the wavelength results in a large change of the effective group propagation angle and therefore of the beam exit position for light beams of oblique incidence angle. Here we demonstrate that such a structure also exhibits a large change in the exit position for a fixed incident wavelength due to a small refractive index variation. We investigate theoretically the introduction of optically nonlinear polymer layers into multilayer thin-film structures for electro-optic switching of the refractive index. Polymers offer a number of advantages as nonlinear materials - they are simple to process, they show high, non-resonant nonlinear coefficients and they posses low refractive indices. A dispersive thin-film stack containing tunable polymer layers is therefore promising as a 1:N spatial beam switch with switching times in the nanosecond range. We developed and simulated different designs for dispersive thin-film stacks consisting of dielectric and polymer layers. The approaches range from Bragg stacks with two alternating materials, one of them the active polymer, over impedance matched Bragg stacks to coupled cavities that contain the active material. The achievable refractive index changes with guest-host polymer systems were evaluated and integrated into our calculations.
Preparation and characterization of multilayers for EUV applications
Th. Foltyn, S. Braun, W. Friedrich, et al.
The dependency of EUV reflectance and of the stress present in Mo/Si/C multilayers on the constituent individual layers has been investigated. The heat treatment of highly EUV reflective Mo/Si/C multilayers has been examined in terms of annealing time and temperature. Irreversible stress change was found at annealing temperatures above 130 °C, where the change of period thickness and the change of stress increase more rapidly. It was found, that there is a saturation of stress change depending on the annealing time. Annealing at 100 °C reveals a saturation of stress change after 10 h, whereas annealing at 150 °C still shows stress reduction after 50 h. A second annealing of two samples shows a reversible stress-temperature behavior of the multilayers. Stress compensation layers for the coating of stress-mitigated Mo/Si/C multilayers were developed. The best results of composition for reflective multilayers and stress-compensation multilayers were joint together in order to fabricate stress-mitigated Mo/Si/C multilayers. Taking the condition of achieving an overall stress below ±100-150 MPa into account, two types of stress-mitigated multilayers were coated. The first type includes a buffer layer in order to compensate the compressive stress of the reflective multilayers without annealing. The stress was reduced to -76 MPa by keeping a high EUV near-normal incidence reflectance of ~70.0 %. The second type contains a thinner buffer layer and the stress reduction of the complete multilayer system was assisted by a post-annealing at 100 °C for 10 h. The stress was measured to be -108 MPa and an EUV reflectance of 69.5 % was obtained.
Genetic algorithm design of reflection thin-film coatings and polarization-devices
A. R. M. Zaghloul, Y. A. Zaghloul
In this communication, the design of reflection thin-film coatings and polarization-devices is achieved by the use of a recently developed fast genetic algorithm (GA). The reflection thin-film coatings, and polarization-devices, are both treated as film-substrate systems. With the required polarization-characteristics of the device as an input, the GA provides any, or all, of the design parameters at which the coating, or device, behaves as prescribed at the wavelength of operation; film and substrate materials, film thickness, and angle of incidence. The GA is real fast. It is modified to provide the required design parameters within a few cycles, literally in no time. The accuracy of the GA is high, and the GA itself is robust and consistent.
High reflectivity measurement with cavity ring-down technique
Li-feng Gao, Sheng-ming Xiong, Bin-cheng Li, et al.
Cavity Ring-Down Spectroscopy (CRDS) is a highly sensitive loss measurement technique. It was used for quantitative diagnostics of molecular species. In our experiment CRDS has been applied for measuring the reflectivities of optical mirrors. An experimental system has been established. The reflectivities of a pair of cavity mirrors and of a 22.5° optical mirror have been measured. The reflectivities of the cavity mirrors are (99.925±0.001) % and that of the 22.5° mirror is (99.992±0.003) %° The measurement error was as low as 0.001%.
Characterization of optical thin films exhibiting defects
In this paper the mathematical formalism enabling us to include defects of thin films into the formulae expressing their optical quantities is presented. The attention is devoted to the defects consisting in boundary roughness and inhomogeneity corresponding to the refractive index profile. This mathematical formalism is based on 2x2 matrix algebra. The Rayleigh-Rice theory (RRT) is used for describing boundary roughness. The refractive index profile is included into the matrix formalism by means a special procedure based on combination of the Drude and Wentzel-Kramers-Brillouin-Jeffries (WKBJ) approximations. The mathematical formalism is applied for the optical characterization of thin films of TiO2 and As-S chalcogenides. Using this formalism the experimental data corresponding to the ellipsometric quantities, reflectance measured from the ambient side, reflectance measured from the substrate side and transmittance are treated. The corrections of the systematic errors connected with the reflection accessory of the spectrometer used is carried out using the special procedure.
Additional Paper from Session on XUV Coatings
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Study of potential quantization effects in designs for 12.4 nm mirrors
Mirrors at normal incidence have been successfully made for the 12.4 nm spectral region using molybdenum (Mo), silicon (Si), and other materials. At these wavelengths, a typical layer is of the order of 3 nm in physical thickness, and the atomic diameters of the materials are of the order of 0.3 nm. The implication is that the layers are of the order of 10 atomic layers thick. If the deposition of such films were done by atomic layer epitaxy (ALE) or other atomic layer deposition (ALD) techniques, the spectral results would fall in discrete patterns that could limit the potential design choices. The problem would be even more severe at shorter wavelengths. This work reports on the study of some of those possibilities and limitations.