Comparison of TiO2 and ZrO2 Films Deposited by Electron-Beam Evaporation and by Sol-Gel Process

TiO2 and ZrO2 films are deposited by electron-beam （EB） evaporation and by sol-gel process. The film properties are characterized by visible and Fourier-transform infrared spectrometry, x-ray diffraction analysis, surface roughness measure, absorption and laser-induced damage threshold （LIDT） test. It is found that the sol-gel films have lower refractive index, packing density and roughness than EB deposited films due to their amorphous structure and high OH group concentration in the film. The high LIDT of sol-gel films is mainly due to their amorphous and porous structure, and low absorption. LIDT of EB deposited film is considerably affected by defects in the film, and LIDT of sol-gel deposited film is mainly effected by residual organic impurities and solvent trapped in the film.     

Effects of annealing on laser-induced damage threshold of TiO2/SiO2 high reflectors

The mechanism of improving 1064 nm, 12 ns laser-induced damage threshold (LIDT) of TiO₂/SiO₂ high reflectors (HR) prepared by electronic beam evaporation from 5.1 to 13.1 J/cm² by thermal annealing is discussed. Through optical properties, structure and chemical composition analysis, it is found that the reduced atomic non-stoichiometric defects are the main reason of absorption decrease and LIDT rise after annealing. A remarkable increase of LIDT is found at 300 °C annealing. The refractive index and film inhomogeneity rise, physical thickness decrease, and film stress changes from compress stress to tensile stress due to the structure change during annealing.     

Effect of Process Parameters on Laser Damage Threshold of TiO2 Coatings

We investigate the laser damage behaviour of an electron-beam-deposited TiO2 monolayer at different process parameters. The optical properties, chemical composition, surface defects, absorption and laser-induced damage threshold （LIDT） of films are measured. It is found that TiO2 films with the minimum absorption and the highest LIDT can be fabricated using a TiO2 starting material after annealing. LIDT is mainly related to absorption and is influenced by the non-stoichiometric defects for TiO2 films. Surface defects show no evident effects on LIDT in this experiment.     

Properties of Cu film and Ti/Cu film on polyimide prepared by ion beam techniques

Cu film and Ti/Cu film on polyimide substrate were prepared by ion implantation and ion beam assisted deposition (IBAD) techniques. Three-dimension white-light interfering profilometer was used to measure thickness of each film. The thickness of the Cu film and Ti/Cu film ranged between 490 nm and 640 nm. The depth profile, surface morphology, roughness, adhesion, nanohardness, and modulus of the Cu and Ti/Cu films were measured by scanning Auger nanoprobe (SAN), atomic force microscopy (AFM), and nanoindenter, respectively. The polyimide substrates irradiated with argon ions were analyzed by scanning electron microscopy (SEM) and AFM. The results suggested that both the Cu film and Ti/Cu film were of good adhesion with polyimide substrate, and ion beam techniques were suitable to prepare thin metal film on polyimide.     

Fabrication of multilayer thin film filters by hydrofluoric acid bonding

A hydrofluoric acid (HF) bonding technique for multilayer thin films was studied to fabricate dielectric multilayer interference filters. The effects of pressure, HF concentration and annealing treatment on bonding strength were studied. Bonding strength of multilayer thin films of more than 5 MPa were obtained. In addition, a new type edge filter of 47 layers (47L) and a band-pass filter of 63 layers (63L), with their films sandwiched between glass substrates, were fabricated using this method. The measured transmittance spectra agreed well with the designed ones.     

Development in Laser Induced Extrinsic Absorption Damage Mechanism of Dielectric Films

Absorption of host and the temperature-dependence of absorption coefficient have been considered in evaluating temperature distribution in films, when laser pulse irradiates on films. Absorption of dielectric materials experience three stages with the increase of temperature： multi-photon absorption; single photon absorption; metallic absorption. These different absorption mechanisms correspond to different band gap energies of materials, which will decrease when the temperature of materials increases. Evaluating results indicate that absorption of host increases rapidly when the laser pulse will be over. If absorption of host and the temperature-dependence of absorption are considered, the maximal temperatures in films will be increased by a factor of four.     

Influence of Vacuum Organic Contaminations on Laser-Induced Damage of 1064 nm Anti-Reflective Coatings

We investigate the influence of vacuum organic contaminations on laser-induced damage threshold （LIDT） of optical coatings. Anti-reflective （AIR） coatings at 1064 nm made by Ta2 O5/SiO2 are deposited by the ion beam sputtering method. The LIDTs of AR coatings are measured in vacuum and in atmosphere, respectively. It is exhibited that contaminations in vacuum are easily to be absorbed onto optical surface because of lower pressure, and they become origins of damage, resulting in the decrease of LIDT from 24.5J/cm^2 in air to 15.TJ/cm^2 in vacuum. The LIDT of coatings in vacuum has is slightly changed compared with the value in atmosphere after the organic contaminations are wiped off. These results indicate that organic contaminations are the main reason of the LIDT decrease in vacuum. Additionally, damage morphologies have distinct changes from vacuum to atmosphere because of the differences between the residual stress and thermal decomposability of filmy materials.     

Fabrication and Characterization of Multi-layer Heat Mirror with Photocatalytic Properties

A novel TiO2（5）/TiO2（buffer）/Ti（4）/Ag（3）/Ti（2）/TiO2（1） multi-layer film coating with corning glass is designed and fabricated by a dc magnetron sputtering method as a renovation of the well-known TiO2/Ti/Ag/Ti/TiO2 system in order to obtain a heat mirror system with photocatalytic properties due to sufficient thickness of the Ti02 layer. The outer TiO2 layer is fabricated in two steps, possibly claimed as two layers TiO2（5） and TiO2（buuer）, among which TiO2（buffer） the 70-nm-thick layer deposited in poor oxygen effectively minimizes the oxidation toward its neighbor Ti（4） layer. The optimal total thickness of the TiO2（5） and TiO（buffer） di-layer is found to be 300nm to yield a highly photo-catalytic property of the film without affecting the optical properties considerably. This multi-layer film can transmit light of above 75-85% in the visible spectrum （380 ≤ λ≤ 760 nm） and reflect radiation of above 90% in the infrared spectrum （ λ≥760 nm）. Such multi-layer coatings are strongly recommended not only as promising transparent heat mirrors but also as photo-catalytic films for architectural window coatings.     

Synthesis of molybdenum silicide by both ion implantation and ion beam assisted deposition

Two groups of Mo/Si films were deposited on surface of Si(1 0 0) crystal. The first group of the samples was prepared by both ion beam assisted deposition (IBAD) and metal vapor vacuum arc (MEVVA) ion implantation technologies under temperatures from 200 to 400 °C. The deposited species of IBAD were Mo and Si, and different sputtering Ar ion densities were selected. The mixed Mo/Si films were implanted by Mo ion with energy of 94 keV, and fluence of Mo ion was 5 × 10¹⁶ ions/cm². The second group of the samples was prepared only by IBAD under the same test temperature range. The Mo/Si samples were analyzed by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), sheet resistance, nanohardness, and modulus of the Mo/Si films were also measured. For the Mo/Si films implanted with Mo ion, XRD results indicate that phase of the Mo/Si films prepared at 400 and 300 °C was pure MoSi₂. Sheet resistance of the Mo/Si films implanted with Mo ion was less than that of the Mo/Si films prepared without ion implantation. Nanohardness and modulus of the Mo/Si films were obviously affected by test parameters.     

Thickness dependence on thermal stability of sputtered Ag nanolayer on Ti/Si(1 0 0)

Thermal stability of Ag layer on Ti coated Si substrate for different thicknesses of the Ag layer have been studied. To do this, after sputter-deposition of a 10 nm Ti buffer layer on the Si(1 0 0) substrate, an Ag layer with different thicknesses (150-5 nm) was sputtered on the buffer layer. Post annealing process of the samples was performed in an N₂ ambient at a flow rate of 200 ml/min in a temperature range from 500 to 700 °C for 30 min. The electrical property of the heat-treated multilayer with the different thicknesses of Ag layer was examined by four-point-probe sheet resistance measurement at the room temperature. Phase formation and crystallographic orientation of the silver layers were studied by θ-2θ X-ray diffraction analysis. The surface topography and morphology of the heat-treated films were determined by atomic force microscopy, and also, scanning electron microscopy. Four-point- probe electrical measurement showed no considerable variation of sheet resistance by reducing the thickness of the annealed Ag films down to 25 nm. Surface roughness of the Ag films with (1 1 1) preferred crystallographic orientation was much smaller than the film thickness, which is a necessary condition for nanometric contact layers. Therefore, we have shown that the Ag layers with suitable nano-thicknesses sputtered on 10 nm Ti buffer layer were thermally stable up to 700 °C.     

Thermal stability of nanoscale silver metallization in Ag/W/Co/Si(1 0 0) multilayer

In this work, we have studied thermal stability of nanoscale Ag metallization and its contact with CoSi₂ in heat-treated Ag(50 nm)/W(10 nm)/Co(10 nm)/Si(1 0 0) multilayer fabricated by sputtering method. To evaluate thermal stability of the systems, heat-treatment was performed from 300 to 900 °C in an N₂ ambient for 30 min. All the samples were analyzed by four-point-probe sheet resistance measurement (R_s), Rutherford backscattering spectrometry (RBS), X-ray diffractometry (XRD), and atomic force microscopy (AFM). Based on our data analysis, no interdiffiusion, phase formation, and R_s variation was observed up to 500 °C in which the Ag layer showed a (1 1 1) preferred crystallographic orientation with a smooth surface and R_s of about 1 Ω/□. At 600 °C, a sharp increase of R_s value was occurred due to initiation of surface agglomeration, WSi₂ formation, and interdiffusion between the layers. Using XRD spectra, CoSi₂ formed at the Co/Si interface preventing W silicide formation at 750 and 800 °C. Meantime, RBS analysis showed that in this temperature range, the W acts as a cap layer, so that we have obtained a W encapsulated Ag/CoSi₂ contact with a smooth surface. At 900 °C, the CoSi₂ layer decomposed and the layers totally mixed. Therefore, we have shown that in Ag/W/Co/Si(1 0 0) multilayer, the Ag nano-layer is thermally stable up to 500 °C, and formation of W-capped Ag/CoSi₂ contact with R_s of 2 Ω/□ has been occurred at 750-800 °C.     

Narrow band filters in both transmission and reflection with metal/dielectric thin films

We present a novel narrow band filter operating in both transmission and reflection for the first time to our knowledge. This proposed structure consists of one unsymmetrical dielectric Fabry-Perot cavity and an ultrathin metal film with n ≈ k. Theoretical analysis shows that both the reflectance and transmittance at the central wavelength are maximums. Due to the high absorption induced by the metal, a good rejection level can be obtained for a wide spectral range. In addition, the changes of peak value ratio R_max/T_max is also investigated by adjusting the amount of dielectric stacks. We finally demonstrate the experimental results to verify these designs.     

Impact of organic contamination on laser-induced damage threshold of high reflectance coatings in vacuum

The influence of organic contamination in vacuum on the laser-induced damage threshold (LIDT) of coatings is studied. TiO₂/SiO₂ dielectric mirrors with high reflection at 1064 nm are deposited by the electron beam evaporation method. The LIDTs of mirrors are measured in vacuum and atmosphere, respectively. It is found that the contamination in vacuum is easily attracted to optical surfaces because of the low pressure and becomes the source of damage. LIDTs of mirrors have a little change in vacuum compared with in atmosphere when the organic contamination is wiped off. The results indicate that organic contamination is a significant reason to decrease the LIDT. N₂ molecules in vacuum can reduce the influence of the organic contaminations and prtectect high reflectance coatings.     

High accuracy measurement of the residual air gap thickness of thin-film and solid-spaced filters assembled by optical contacting

Optical contacting is a powerful tool for assembling solid-spaced filters in order to form a wavelength division multiplexing (WDM) multiple-cavity filter. In this article, we propose a method able to characterize the optical quality of such assembling with a high accuracy. We use localized spectral transmittance measurements to map the thickness of the residual air gap existing at the adhesion interface with a few nanometers precision. Tests on thick (2 mm) and thin (100 μm) substrates coated by Dual Ion Beam Sputtering are performed. Thus, we show that our 25 mm-diameter samples are strictly contacted over more than 80% of their surface, with no detectable residual air gap.     

Intrinsic stress of ultrathin epitaxial films

The present article focuses on the stress developing during the deposition of ultrathin epitaxial films in the thickness range of a few atomic layers. The studied systems exhibit the three well-known modes of film growth: Stranski–Krastanow mode [Ge/Si(001), Ge/Si(111), Ag/Si(111)], Frank–Van der Merwe mode [Fe/MgO(001)] and Volmer–Weber mode [Ag/mica(001), Cu/mica(001)]. The experimental results demonstrate the important role of the misfit strain as well as the contribution of surface stress effects as mechanisms for the stress in single atomic layers. Received: 26 April 1999 / Accepted: 25 June 1999 / Published online: 6 October 1999     

Studies of the promising material CoSi2 on GaAs substrates

The thermal stability of CoSi₂ thin films on GaAs substrates has been studied using a variety of techniques. The CoSi₂ thin films were formed by depositing Co(500 Å) and Si(1800 Å) layers on GaAs substrates by electron-beam evaporation followed by annealing processes, where the Si inter-layer was used as a diffusion/reaction barrier at the interface. The resistivity of CoSi₂ thin films formed is about 30 cm. The Schottky barrier height of CoSi₂/n-GaAs is 0.76 eV and the ideality factor is 1.14 after annealing at 750° C for 30 min. The CoSi₂/GaAs interface is determined to be thermally stable and the thin film morphologically uniform on GaAs after 900° C/30 s anneal. The CoSi₂ thin films fulfill the requirements in GaAs self-aligned gate technology.     

Surface flatness of optical thin films evaluated by gray level co-occurrence matrix and entropy

The surface characteristics of titanium oxide films evaluated by gray level co-occurrence matrices (GLCMs) and entropy are demonstrated experimentally. A PC-based measurement system was set up to detect the interference fringe of optical coating surface as captured by a Fizeau interferometer. Titanium oxide films were prepared by an electron-beam gun evaporation method. The proposed measuring system was used to evaluate the surface flatness of titanium oxide films coated on glass substrates. The variation of entropy in titanium oxide films before and after film deposition was found to be related to the root-mean-square (rms) surface roughness. Surface characteristics of thin films were fast measured by our proposed method and the test results were verified by atomic force microscopy (AFM) and scanning electrical microscopy (SEM).     

Fabrication of atomic gratings based on self-organization of adsorbates with repulsive interaction

Received: 5 May 1997/Accepted: 6 May 1997     

Fabrication of pellicle beam splitters for optical bus application

The optical bus architecture for on-board applications requires a number of optical splitters with precise split ratios to route part of the input signal. Since hollow metal waveguide provides well collimated beams with very small gap loss, it opens the possibility of inserting discrete optical beam splitters (taps). The optical tap requires low excess loss, polarization insensitivity, temperature stability, minimized walk-off of the propagating beam, and cost effective manufacturing. By benefiting from the mature interference coating technology for polarization insensitivity and temperature stability, we design a pellicle beam splitter based on a static microelec tro-mechanical system (MEMS) and develop processes to fabricate pellicle splitters using wafer level bonding of silicon and glass substrates, with subsequent thinning to 20 μm. With the approaches described in this paper, we have demonstrated optical beam splitters with excess loss of less than 0.17 dB that operate at a data rate of 10 Gb/s showing a clean eye diagram while providing controlled split ratio and polarization insensitivity. We have demonstrated a high yielding MEMS based silicon processing platform which has the potential to provide a cost effective manufacturing solution for optical beam splitters.     

Elastic modulus-density relationship for amorphous boron suboxide thin films

Boron suboxide thin films have been deposited on Si(100) substrates by reactive RF magnetron sputtering of a sintered B target in an Ar/O₂ atmosphere. Elastic recoil detection analysis was applied to determine the film composition and density. Film structure was studied by X-ray diffraction and transmission electron microscopy. The elastic modulus, measured by nanoindentation, was found to decrease as the film density decreased. The relationship was affected by tuning the negative substrate bias potential and the substrate temperature during film growth. A decrease in film density, by a factor of 1.55, caused an elastic modulus reduction by a factor of 4.5, most likely due to formation of nano-pores containing Ar. It appears evident that the large scattering in the published data on elastic properties of films with identical chemical composition can readily be understood by density variations. These results are important for understanding the elastic properties of boron suboxide, but may also be qualitatively relevant for other B-based material systems. Received: 22 February 2002 / Accepted: 11 April 2002 / Published online: 10 September 2002 RID="*" ID="*"Corresponding author. Fax: +46-13/288-918, E-mail: denmu@ifm.liu.se