Richard Vernhes

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...

Plasma treatment of porous SiNx:H films for the fabrication of porous-dense multilayer optical filters with tailored interfaces

Porous and dense silicon nitride films with low (1.58) and high (1.88) refractive indices were prepared by using successively microwave and radio frequency (rf) plasma-enhanced chemical vapor deposition. Surface treatments were performed on porous layers using argon and nitrogen rf plasmas in order to densify and flatten their surface, and hence to obtain an abrupt transition between porous and dense films. The processes during deposition and interface treatment were studied by in situ real-time spectroscopic ellipsometry as well as by other characterization techniques. We show that besides the densification effect, preferential sputtering and annealing phenomena occur during plasma treatments at high bias (∣VBtreat∣>400V), leading to silicon enrichment at the film surface and chemical stabilization of the film bulk. Using atomic force microscopy, we observed a significant reduction of the thickness of the surface roughness layer after treatment for single layers (≈70% reduction) and multilayer stacks (≈6...

Reactive HiPIMS deposition of SiO2/Ta2O5 optical interference filters

In this contribution, based on the detailed understanding of the processes at the target during reactive high power impulse magnetron sputtering (HiPIMS), we demonstrate the deposition of both low- and high-index films and their implementation in optical interference filters with enhanced performance. We first investigate strategies for stabilizing the arc-free HiPIMS discharges above Si and Ta targets in the presence of oxygen. We show that hysteresis can be suppressed for these two target materials by suitable pulse-management strategies, ensuring good process stability without having to rely on any feedback control. Afterwards, we discuss the room temperature deposition of optically transparent SiO2 and Ta2O5 single layers as well as the fabrication of SiO2/Ta2O5 stacks such as 7 layer Bragg reflectors and 11 layer Fabry-Perot interference filters. We also analyze the optical and mechanical characteristics of these various coatings and compare them with their counterparts obtained by radio-frequency ma...

Galvanostatic Rejuvenation of Electrochromic WO3 Thin Films: Ion Trapping and Detrapping Observed by Optical Measurements and by Time-of-Flight Secondary Ion Mass Spectrometry

Electrochromic (EC) smart windows are able to decrease our energy footprint while enhancing indoor comfort and convenience. However, the limited durability of these windows, as well as their cost, result in hampered market introduction. Here, we investigate thin films of the most widely studied EC material, WO3. Specifically, we combine optical measurements (using spectrophotometry in conjunction with variable-angle spectroscopic ellipsometry) with time-of-flight secondary ion mass spectrometry and atomic force microscopy. Data were taken on films in their as-deposited state, after immersion in a Li-ion-conducting electrolyte, after severe degradation by harsh voltammetric cycling and after galvanostatic rejuvenation to regain the original EC performance. Unambiguous evidence was found for the trapping and detrapping of Li ions in the films, along with a thickness increase or decrease during degradation and rejuvenation, respectively. It was discovered that (i) the trapped ions exhibited a depth gradient; (ii) following the rejuvenation procedure, a small fraction of the Li ions remained trapped in the film and gave rise to a weak short-wavelength residual absorption; and (iii) the surface roughness of the film was larger in the degraded state than in its virgin and rejuvenated states. These data provide important insights into the degradation mechanisms of EC devices and into means of achieving improved durability.

TRACK--A new method for the evaluation of low-level extinction coefficient in optical films.

We develop a rigorous methodology named TRACK based on the collection of multi-angle spectrophotometric transmission and reflection data in order to assess the extinction coefficient of quasi-transparent optical films. The accuracy of extinction coefficient values obtained by this method is not affected by sample non-idealities (thickness non-uniformity, refractive index inhomogeneities, anisotropy, interfaces, etc.) and therefore a simple two-layer (substrate/film) optical model can be used. The method requires the acquisition of transmission and reflection data at two angles of incidence: 10° and 65° in p polarization. Data acquired at 10° provide information about the film thickness and the refractive index, while data collected at 65° are used for absorption evaluation and extinction coefficient computation. We test this method on three types of samples: (i) a CR-39 plastic substrate coated with a thick protective coating; (ii) the same substrate coated with a thin TiO(2) film; (iii) and a thick Si(3)N(4) film deposited on Gorilla glass that presents thickness non-uniformity and refractive index gradient non-idealities. We also compare absorption and extinction coefficient values obtained at 410 and 550 nm by both TRACK and Laser Induced Deflection techniques in the case of a 1 micron thick TiO(2) coating. Both methods display consistent extinction coefficient values in the 10(-4) and 10(-5) ranges at 410 and 550 nm, respectively, which proves the validity of the methodology and provides an estimate of its accuracy limit.

Hard AlN films prepared by low duty cycle magnetron sputtering and by other deposition techniques

Crystalline AlN films are very attractive due to their properties such as high thermal stability and relatively high hardness and piezoelectric response. However, the deposition of dense textured AlN films with superior quality at a high deposition rate remains a challenge. In the present work, a reactive low duty cycle pulsed direct current magnetron sputtering (LDMS) process was employed to deposit AlN films on glass and silicon substrates. An arc-free discharge on the Al target was achieved by using short voltage pulses of 10 μs at a low duty cycle of 10%. The authors optimized the deposition conditions in terms of reactive gas flow, working pressure, average target power, substrate temperature, substrate bias, and the level of target erosion. With the optimized deposition conditions, the authors were able to obtain transparent crystalline AlN films with strong (002) preferential orientation and very good optical and mechanical properties: The AlN films with the highest refractive index of 2.1 present ...

Ellipsometric monitoring of the refractive index evolution versus temperature for various metal oxides commonly used in interference filters

The optical properties of room temperature sputter-deposited metal oxide films on fused silica substrates are investigated by in situ spectroscopic ellipsometry over a wide temperature range.

Durable AlN and Al 2 O 3 Optical Films Deposited by Low Duty Cycle Pulsed Magnetron Sputtering

We applied low-duty cycle pulsed magnetron reactive sputtering of an Al target to achieve stable deposition of transparent Al2O3 films and AlN films with high density, high hardness, and low stress at deposition rates of ~60 nm/min.

Optical and electrical characteristics of transparent and highly conductive ultrathin nickel films

Smooth ultrathin transparent conductive Ni films were fabricated by radio frequency sputtering at room temperature. A novel method based on angle resolved transmittance and reflectance measurements allowed calculation of films optical constants.