Oleg Zabeida

Optical properties and microstructure of plasma deposited Ta2O5 and Nb2O5 films

Advanced optical filter applications require an appropriate control of the optical constants, as well as of other suitable film properties such as mechanical performance, thermal and environmental stability, absence of refractive index inhomogeneities, and others. In the present work we studied the characteristics of two high index optical materials, namely amorphous tantalum pentoxide (Ta2O5) and niobium pentoxide (Nb2O5) prepared by plasma enhanced chemical vapor deposition, using penta-ethoxy tantalum Ta(OC2H5)5 and penta-ethoxy niobium, Nb(OC2H5)5, precursors. We particularly investigated the effect of energetic conditions on the film growth by using different modes of plasma excitation, namely rf, microwave, and dual-mode microwave/radio frequency discharges. Under sufficient ion bombardment, controlled by the rf-induced negative substrate bias, the dense Ta2O5 and Nb2O5 films exhibited a refractive index of 2.16 and 2.26 (at 550nm), respectively, while the extinction coefficient was below 10−5, as d...

Dynamics of reactive high-power impulse magnetron sputtering discharge studied by time- and space-resolved optical emission spectroscopy and fast imaging

Time- and space-resolved optical emission spectroscopy and fast imaging were used for the investigation of the plasma dynamics of high-power impulse magnetron sputtering discharges. 200 μs pulses with a 50 Hz repetition frequency were applied to a Cr target in Ar, N2, and N2/Ar mixtures and in a pressure range from 0.7 to 2.66 Pa. The power density peaked at 2.2–6 kW cm−2. Evidence of dominating self-sputtering was found for all investigated conditions. Up to four different discharge phases within each pulse were identified: (i) the ignition phase, (ii) the high-current metal-dominated phase, (iii) the transient phase, and (iv) the low-current gas-dominated phase. The emission of working gas excited by fast electrons penetrating the space in-between the electrodes during the ignition phase spread far outwards from the target at a speed of 24 km s−1 in 1.3 Pa of Ar and at 7.5 km s−1 in 1.3 Pa of N2. The dense metal plasma created next to the target propagated in the reactor at a speed ranging from 0.7 to 3...

Hysteresis-free deposition of niobium oxide films by HiPIMS using different pulse management strategies

We systematically investigate the reactive behaviour of two types of high-power pulsed magnetron discharges above a Nb target using either square voltage pulses (denoted as HiPIMS) or custom-shaped pulses (denoted as MPPMS), and compare it with that of a dc magnetron sputtering (DCMS) discharge. We demonstrate that the surface metal oxides can be effectively sputter-eroded from the target during both HiPIMS and MPPMS pulses operated in reactive O2/Ar gas mixtures, and that sputtering from a partially oxide-free target is possible even at high oxygen concentrations. This results in a hysteresis-free deposition process which allows one to prepare optically transparent high refractive index Nb2O5 coatings exhibiting an elevated deposition rate without the need for feedback control commonly used in reactive DCMS. The cathode voltage was identified as the principal parameter that affects the reactive discharge behaviour.

Deposition rate enhancement in HiPIMS without compromising the ionized fraction of the deposition flux

We systematically investigate and quantify different physical phenomena influencing the deposition rate, aD, of Nb coatings prepared by high power impulse magnetron sputtering (HiPIMS), and propose a straightforward approach for deposition rate enhancement through the control of the magnetrons magnetic field. The magnetic field strength at the target surface, B, of a 50?mm diameter magnetron was controlled by the application of paramagnetic spacers with different thicknesses in between the magnetron surface and the target. We found that lowering B achieved by the application of a 2.8?mm thick spacer led to an increase in aD by a factor of ?4.5 (from 10.6 to 45.2?nm?min?1) when the discharge was operated at a fixed average pulse target power density (2.5?kW?cm?2). However, the ionized fraction of the deposition flux onto the substrate was found to be comparable, despite a large difference in B-dependent discharge characteristics (magnetron voltage and discharge current). We show that the decrease in aD commonly observed in HiPIMS (ranging from 33% to 84% in comparison with dc magnetron sputtering in the presented experiments) is governed by different physical processes, depending on the value of B: for high B, the back-attraction of the target ions towards the target is the dominant effect, while for low B the ion back-attraction, the sub-linear dependence of the sputtering yield on the ion energy, and the variation in material transport effects are all important. Finally, we offer a theoretical background for the observed results, demonstrating that the here-presented conclusions may be applicable to HiPIMS discharges using different metal targets and different inert gases.

Mechanical and thermoelastic characteristics of optical thin films deposited by dual ion beam sputtering.

Mechanical and thermoelastic properties of optical films are very important to ensure the performance of optical interference filters and optical coating systems. We systematically study the growth and the mechanical and thermoelastic characteristics of niobium oxide (Nb(2)O(5)), tantalum oxide (Ta(2)O(5)), and silicon dioxide (SiO(2)) thin films prepared by dual ion beam sputtering. First, we investigate the stress (sigma), hardness (H), reduced Youngs modulus (E(r)), and scratch resistance. Second, we focus on the methodology and assessment of the coefficient of thermal expansion (CTE) and Poissons ratio (nu) using the two-substrate method. For the high refractive index films, namely, Nb(2)O(5) (n at 550 nm=2.30) and Ta(2)O(5) (n at 550 nm=2.13), we obtained H approximately 6 GPa, E(r) approximately 125 GPa, CTE=4.9x10(-6) degrees C(-1), nu=0.22, and H approximately 7 GPa, E(r) approximately 133 GPa, CTE=4.4x10(-6) degrees C(-1), and nu=0.27, respectively. In comparison, for SiO(2) (n at 550 nm=1.48), these values are H approximately 9.5 GPa, E(r) approximately 87 GPa, CTE=2.1x10(-6) degrees C(-1), and nu=0.11. Correlations between the growth conditions (secondary beam ion energy and ion current), the microstructure, and the film properties are discussed.

Single-material inhomogeneous optical filters based on microstructural gradients in plasma-deposited silicon nitride

Transparent hydrogenated amorphous silicon nitride (SiNx:H) coatings were prepared by dual-mode microwave-radio-frequency plasma-enhanced chemical vapor deposition. By controlling the effects of plasma density and ion energy on the film growth, it was possible to modify the microstructure of the coatings and hence the refractive index n. Using this method, we were able to vary n from 1.6 to 2.0, at 550 nm, by adjusting the power levels of the radio-frequency and microwave components while keeping the gas composition (SiH4, N2) and pressure constant. An inhomogeneous bandpass filter with a controlled refractive-index depth profile was fabricated, and its optical performance was compared with that of its multilayer counterpart. Besides the attractive optical features of such single-material rugate filters, we found that the mechanical resistance of inhomogeneous films is superior to that of multilayer systems.

Pulsed radio frequency plasma deposition of a-SiNx:H alloys: Film properties, growth mechanism, and applications

In this work, we propose a fabrication process of a-SiNx:H alloys by pulsing the radio frequency (rf) signal in a low pressure plasma-enhanced chemical vapor deposition (PECVD) system. The characteristics of the films can be controlled simply by adjusting the duty cycle of the pulsed rf power, while keeping the N2∕SiH4 gas mixture constant. Spectroscopic ellipsometry analysis in the ultraviolet-visible-near infrared and far infrared ranges, atomic force microscopy, and elastic recoil detection reveal strong variations in the optical properties (1.88⩽n⩽2.75, 10−4⩽k⩽5×10−2 at 550nm), optical gap (4.01eV⩽Eg⩽1.95eV), microstructural characteristics (1.3nm⩽surfaceroughness⩽8.3nm), and chemical composition (0.47⩽x⩽1.35) of the coatings as a function of duty cycle. This behavior is interpreted in terms of radical concentration changes in the gas phase, as well as variation in the average ion bombardment energy at the film surface, leading to modifications of both chemical and physical mechanisms that sustain the...

Mass-resolved ion energy distributions in continuous dual mode microwave'radio frequency plasmas in argon and nitrogen

The control of plasma-surface interactions in terms of synergistic effects of ions, photons, and chemically active species is important for the optimization of plasma enhanced chemical vapor deposition of thin films and for plasma-induced surface modification. In the present work, we use a dual-mode microwave/radio frequency (MW/rf) plasma system, in which we investigate the effect of plasma parameters (gas type and pressure, self-bias voltage, for example) on the energy and flux of ionic species arriving at the specimen surface. We determine the ion energy distribution functions (IEDFs) using a mass spectrometer/energy analyzer, in Ar and N2 discharges, excited at different frequencies. The results for Ar+, N2+, and N+ ions show structured IEDFs at the rf-powered electrode in the single- and dual-frequency modes, while a single peak is observed in the continuous MW plasma. The MW/rf plasma presents substantially higher ion flux and plasma density, and a much thinner sheath than the rf case. Changes in pl...

Time-resolved measurements of ion energy distributions in dual-mode pulsed-microwave/radio frequency plasma

In the present work we systematically study the ion energy distribution functions (IEDFs) in argon discharges produced by a combination of pulsed (1–2 kHz) microwave (MW) and continuous wave (cw) radio frequency (rf) excitations. We show that the IEDFs for the pulsed MW discharges are structured, with individual features originating from different periods of the pulse. In the dual-mode MW/rf discharge, significant modulation of the self-bias voltage, Vb, during the MW pulse cycle is observed, which we attribute to changes in the overall plasma impedance: We demonstrate that in the pulsed-MW/cw-rf mode the impedance is highly resistive when the MW signal is on, while it is predominantly capacitive during the period between individual pulses. Using the measured time evolution of Vb in combination with time-resolved measurements of individual ion species, IEDFs at the rf-powered electrode at each instant of the MW pulse have been obtained. This approach is then used to reconstruct the total IEDF in pulsed-MW...

Steady state discharge optimization in high-power impulse magnetron sputtering through the control of the magnetic field

High-power impulse magnetron sputtering (HiPIMS) is a pulsed DC sputtering technique utilizing high power density peaks of typically more than 100 W cm−2. The discharge operation at such elevated powers can be hindered by the magnetron configuration (size and magnetic field) and/or the target conditions (e.g., material and thickness). In addition, target erosion is an important issue significantly affecting process reproducibility. In the present work, we propose a simple approach for the stabilization of the HiPIMS discharge by controlling the target magnetic field using paramagnetic spacers with different thicknesses in between the magnetron surface and the target. We demonstrate a straightforward discharge optimization, while using various target materials, such as Nb, Ta, Cr, Al, Ti, Si, and even C (graphite). The existence of a steady state high density discharge above the graphite target and the other targets in general is discussed in terms of the magnetic field configuration and the gas rarefactio...