X-ray mirrors with sub-nanometre figure errors obtained by differential deposition of thin WSi2 films.

Differential deposition by DC magnetron sputtering was applied to correct for figure errors of X-ray mirrors to be deployed on low-emittance synchrotron beamlines. During the deposition process, the mirrors were moved in front of a beam-defining aperture and the required velocity profile was calculated using a deconvolution algorithm. The surface figure was characterized using conventional off-line visible-light metrology instrumentation (long trace profiler and Fizeau interferometer) before and after the deposition. WSi2 was revealed to be a promising candidate material since it conserves the initial substrate surface roughness and limits the film stress to acceptable levels. On a 300 mm-long flat Si mirror the average height errors were reduced by a factor of 20 down to 0.2 nm root mean square. This result shows the suitability of WSi2 for differential deposition. Potential promising applications include the upgrade of affordable, average-quality substrates to the standards of modern synchrotron beamlines.

Sputter Deposited Magnetostrictive Layers for SAW Magnetic Field Sensors.

For the best possible limit of detection of any thin film-based magnetic field sensor, the functional magnetic film properties are an essential parameter. For sensors based on magnetostrictive layers, the chemical composition, morphology and intrinsic stresses of the layer have to be controlled during film deposition to further control magnetic influences such as crystallographic effects, pinning effects and stress anisotropies. For the application in magnetic surface acoustic wave sensors, the magnetostrictive layers are deposited on rotated piezoelectric single crystal substrates. The thermomechanical properties of quartz can lead to undesirable layer stresses and associated magnetic anisotropies if the temperature increases during deposition. With this in mind, we compare amorphous, magnetostrictive FeCoSiB films prepared by RF and DC magnetron sputter deposition. The chemical, structural and magnetic properties determined by elastic recoil detection, X-ray diffraction, and magneto-optical magnetometry and magnetic domain analysis are correlated with the resulting surface acoustic wave sensor properties such as phase noise level and limit of detection. To confirm the material properties, SAW sensors with magnetostrictive layers deposited with RF and DC deposition have been prepared and characterized, showing comparable detection limits below 200 pT/Hz1/2 at 10 Hz. The main benefit of the DC deposition is achieving higher deposition rates while maintaining similar low substrate temperatures.

Mitigating Water Absorption in Waveguides Made From Unannealed PECVD SiO2.

Water absorption was studied in two types of waveguides made from unannealed plasma enhanced chemical vapor deposition (PECVD) SiO2. Standard rib anti-resonant reflecting optical waveguides (ARROWs) were fabricated with thin films of different intrinsic stress and indices of refraction. Buried ARROWs (bARROWs) with low and high refractive index differences between the core and cladding regions were also fabricated from the same types of PECVD films. All waveguides were subjected to a heated, high humidity environment and their optical throughput was tested over time. Due to water absorption in the SiO2 films, the optical throughput of all of the ARROWs decreased with time spent in the wet environment. The ARROWs with the lowest stress SiO2 had the slowest rate of throughput change. High index difference bARROWs showed no decrease in optical throughput after 40 days in the wet environment and are presented as a solution for environmentally stable waveguides made from unannealed PECVD SiO2.

A Design Approach to Reducing Stress and Distortion Caused by Adhesive Assembly in Micromachined Deformable Mirrors.

A common problem in deformable mirror assembly is that the adhesion of actuators to an optical mirror face sheet introduces unwanted topography due to large local stresses generated at the adhesive joint. A new approach to minimizing that effect is described, with inspiration taken from St. Venant's principle, a fundamental precept in solid mechanics. It is demonstrated that moving the adhesive joint to the end of a slender post extending from the face sheet largely eliminates deformation due to adhesive stresses. A practical implementation of this design innovation is described, using silicon-on-insulator wafers and deep reactive ion etching. Simulation and experiments validate the effectiveness of the approach, reducing stress-induced topography on a test structure by a factor of 50. A prototype electromagnetic DM using this design approach is described, and its actuation is demonstrated. This new design can benefit a wide range of DMs that rely on actuator arrays that are adhesively bonded to a mirror face sheet.

Evaluation and Optimization of a MOEMS Active Focusing Device.

In this paper we present a detailed evaluation of a micro-opto-electromechanical system (MOEMS) for active focusing which is realized using an electrostatically deformed thin silicon membrane. The evaluation is done using finite element methods and experimental characterization of the device behavior. The devices are realized in silicon on insulator technology. The influence of internal stress especially resulting from the high compressive buried oxide (BOX) layer is evaluated. Additionally, the effect of stress gradients in the crystalline device layer and of high reflective coatings such as aluminum is discussed. The influence of variations of some important process steps on the device performance is quantified. Finally, practical properties such as focal length control, long-term stability, hysteresis and dynamical response are presented and evaluated. The evaluation proves that the proposed membrane focusing device is suitable for high performance imaging (wavefront errors between λ/5-λ/10) with a large aperture (5 mm).

Machine Learning Assisted Classification of Aluminum Nitride Thin Film Stress via In-Situ Optical Emission Spectroscopy Data.

In this study, we submit a complex set of in-situ data collected by optical emission spectroscopy (OES) during the process of aluminum nitride (AlN) thin film. Changing the sputtering power and nitrogen(N2) flow rate, AlN film was deposited on Si substrate using a superior sputtering with a pulsed direct current (DC) method. The correlation between OES data and deposited film residual stress (tensile vs. compressive) associated with crystalline status by X-ray diffraction spectroscopy (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM) measurements were investigated and established throughout the machine learning exercise. An important answer to know is whether the stress of the processing film is compressive or tensile. To answer this question, we can access as many optical spectra data as we need, record the data to generate a library, and exploit principal component analysis (PCA) to reduce complexity from complex data. After preprocessing through PCA, we demonstrated that we could apply standard artificial neural networks (ANNs), and we could obtain a machine learning classification method to distinguish the stress types of the AlN thin films obtained by analyzing XRD results and correlating with TEM microstructures. Combining PCA with ANNs, an accurate method for in-situ stress prediction and classification was created to solve the semiconductor process problems related to film property on deposited films more efficiently. Therefore, methods for machine learning-assisted classification can be further extended and applied to other semiconductors or related research of interest in the future.

Simulative and Experimental Characterization of an Adaptive Astigmatic Membrane Mirror.

Adaptive optical (AO) components play an important role in numerous optical applications, from astronomical telescopes to microscope imaging systems. For most of these AO components, the induced wavefront correction, respectively added optical power, is based on a rotationally symmetric or segmented design of the AO component. In this work, we report on the design, fabrication, and characterization of a micro-electronic-mechanical system (MEMS) adaptive membrane mirror in the shape of a parabolic cylinder. In order to interpret the experimental characterization results correctly and provide a tool for future application development, this is accompanied by the setup of an optical simulation model. The characterization results showed a parabolically deformable membrane mirror with an aperture of 8 × 2 mm2 and an adaptive range for the optical power from 0.3 to 6.1 m-1 (dpt). The optical simulation model, using the Gaussian beamlet propagation method, was successfully validated by laser beam profile measurements taken in the optical characterization setup. This MEMS-based adaptive astigmatic membrane mirror, together with the accompanying simulation model, could be a key component for the rapid development of new optical systems, e.g., adaptive laser line generators.

Fast Organic Vapor Phase Deposition of Thin Films in Light-Emitting Diodes.

Fast deposition of thin films is essential for achieving low-cost, high-throughput phosphorescent organic light-emitting diode (PHOLED) production. In this work, we demonstrate rapid and uniform growth of semiconductor thin films by organic vapor phase deposition (OVPD). A green PHOLED comprising an emission layer (EML) grown at 50 Å/s with bis[2-(2-pyridinyl-N)phenyl-C](acetylacetonato)iridium(III) (Ir(ppy)2(acac)) doped into 4,4'-bis(N-carbazolyl)-1,1'-biphenyl (CBP) exhibits a maximum external quantum efficiency of 20 ± 1%. The morphology, charge transport properties, and radiative efficiency under optical and electrical excitation of the PHOLED EML are investigated as functions of the deposition rate via both experimental and theoretical approaches. The EML shows no evidence for gas phase nucleation of the organic molecules at deposition rates as high as 50 Å/s. However, the roll-off in quantum efficiency at high current progressively increases with deposition rate due to enhanced triplet-polaron annihilation. The roll-off results from accumulation of stress within the PHOLED EML that generates a high density of defect states. The defects, in turn, act as recombination sites for triplets and hole polarons, leading to enhanced triplet-polaron annihilation at high current. We introduce a void nucleation model to describe the film morphology evolution that is observed using electron microscopy.

Cantilever measurements of surface stress, surface reconstruction, film stress and magnetoelastic stress of monolayers.

We review the application of cantilever-based stress measurements in surface science and magnetism. The application of thin (thickness appr. 0.1 mm) single crystalline substrates as cantilevers has been used successfully to measure adsorbate-induced surface stress changes, lattice misfit induced film stress, and magneto-elastic stress of ferromagnetic monolayers. Surface stress changes as small as 0.01 N/m can be readily measured, and this translates into a sensitivity for adsorbate-coverage well below 0.01 of one layer. Stress as large as several GPa, beyond the elasticity limits of high strength materials, is measured, and it is ascribed to the lattice misfit between film and substrate. Our results point at the intimate relation between surface stress and surface reconstruction, stress-induced structural changes in epitaxially strained films, and strain-induced modifications of the magneto-elastic coupling in ferromagnetic monolayers.

In Situ Measurement of Voltage-Induced Stress in Conducting Polymers with Redox-Active Dopants.

Minimization of stress-induced mechanical rupture and delamination of conducting polymer (CP) films is desirable to prevent failure of devices based on these materials. Thus, precise in situ measurement of voltage-induced stress within these films should provide insight into the cause of these failure mechanisms. The evolution of stress in films of polypyrrole (pPy), doped with indigo carmine (IC), was measured in different electrochemical environments using the multibeam optical stress sensor (MOSS) technique. The stress in these films gradually increases to a constant value during voltage cycling, revealing an initial break-in period for CP films. The nature of the ions involved in charge compensation of pPy[IC] during voltage cycling was determined from electrochemical quartz crystal microbalance (EQCM) data. The magnitude of the voltage-induced stress within pPy[IC] at neutral pH correlated with the radius of the hydrated mobile ion in the order Li(+) > Na(+) > K(+). At acidic pH, the IC dopant in pPy[IC] undergoes reversible oxidation and reduction within the range of potentials investigated, providing a secondary contribution to the observed voltage-induced stress. We report on the novel stress response of these polymers due to the presence of pH-dependent redox-active dopants and how it can affect material performance.

SiNx Coatings Deposited by Reactive High Power Impulse Magnetron Sputtering: Process Parameters Influencing the Nitrogen Content.

Reactive high power impulse magnetron sputtering (rHiPIMS) was used to deposit silicon nitride (SiNx) coatings for biomedical applications. The SiNx growth and plasma characterization were conducted in an industrial coater, using Si targets and N2 as reactive gas. The effects of different N2-to-Ar flow ratios between 0 and 0.3, pulse frequencies, target power settings, and substrate temperatures on the discharge and the N content of SiNx coatings were investigated. Plasma ion mass spectrometry shows high amounts of ionized isotopes during the initial part of the pulse for discharges with low N2-to-Ar flow ratios of <0.16, while signals from ionized molecules rise with the N2-to-Ar flow ratio at the pulse end and during pulse-off times. Langmuir probe measurements show electron temperatures of 2-3 eV for nonreactive discharges and 5.0-6.6 eV for discharges in transition mode. The SiNx coatings were characterized with respect to their composition, chemical bond structure, density, and mechanical properties by X-ray photoelectron spectroscopy, X-ray reflectivity, X-ray diffraction, and nanoindentation, respectively. The SiNx deposition processes and coating properties are mainly influenced by the N2-to-Ar flow ratio and thus by the N content in the SiNx films and to a lower extent by the HiPIMS frequencies and power settings as well as substrate temperatures. Increasing N2-to-Ar flow ratios lead to decreasing growth rates, while the N content, coating densities, residual stresses, and the hardness increase. These experimental findings were corroborated by density functional theory calculations of precursor species present during rHiPIMS.

Influence of Carrier Gas Composition on the Stress of Al2O3 Coatings Prepared by the Aerosol Deposition Method.

Al2O3 films were prepared by the aerosol deposition method at room temperature using different carrier gas compositions. The layers were deposited on alumina substrates and the film stress of the layer was calculated by measuring the deformation of the substrate. It was shown that the film stress can be halved by using oxygen instead of nitrogen or helium as the carrier gas. The substrates were annealed at different temperature steps to gain information about the temperature dependence of the reduction of the implemented stress. Total relaxation of the stress can already be achieved at 300 °C. The XRD pattern shows crystallite growth and reduction of microstrain while annealing.