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Blistering is a phenomenon sometimes observed in sputtered-deposited thin films but seldom investigated in detail. Here, we consider the case of titania-doped germania (TGO)/silica multi-layers deposited by ion beam sputtering. TGO is a candidate as high refractive index material in the Bragg mirrors for the next iteration of gravitational waves detectors. It needs to be annealed at 600°C for 100h in order to reach the desired relaxation state. However under some growth conditions, in 52-layer TGO/silica stacks, blistering occurs upon annealing at a temperature near 500°C, which corresponds to the temperature where Ar desorbs from TGO. In order to better understand the blistering phenomenon, we measure the Ar transport in single layers of TGO and silica. In the case of <1 μm-thick TGO layers, the Ar desorption is mainly limited by detrapping. The transport model also correctly predicts the evolution of the total amount of Ar in a 8.5 μm stack of TGO and silica layers annealed at 450°C, but in that case, the process is mainly limited by diffusion. Since Ar diffusion is an order of magnitude slower in TGO compared to silica, we observe a correspondingly strong accumulation of Ar in TGO. The Ar transport model is used to explain some regimes of the blisters growth, and we find indications that Ar accumulation is a driver for their growth in general, but the blisters nucleation remains a complex phenomenon influenced by several other factors including stress, substrate roughness, and impurities.

Annealing of amorphous optical coatings has been shown to generally reduce optical absorption, optical scattering, and mechanical loss, with higher temperature annealing giving better results. The achievable maximum temperatures are limited to the levels at which coating damage, such as crystallization, cracking, or bubbling, will occur. Coating damage caused by heating is typically only observed statically after annealing. An experimental method to dynamically observe how and over what temperature range such damage occurs during annealing is desirable as its results could inform manufacturing and annealing processes to ultimately achieve better coating performance. We developed a new, to the best of our knowledge, instrument that features an industrial annealing oven with holes cut into its sides for viewports to illuminate optical samples and observe their coating scatter and eventual damage mechanismsin situand in real time during annealing. We present results that demonstratein situobservation of changes to titania-doped tantala coatings on fused silica substrates. We obtain a spatial image (mapping) of the evolution of these changes during annealing, an advantage over x ray diffraction, electron beam, or Raman methods. We infer, based on other experiments in the literature, these changes to be due to crystallization. We further discuss the utility of this apparatus for observing other forms of coating damage such as cracking and blisters.

Air annealing generally reduces absorption, scattering, and mechanical loss in amorphous coatings up to temperatures where damage occurs. Our instrument uses an industrial oven with viewports to observe coating scatter and damage during annealing.

Optical coatings formed from amorphous oxide thin films have many applications in precision measurements. The Advanced Laser Interferometer Gravitational-Wave Observatory (LIGO) and Advanced Virgo use coatings of$\mathrm{S}\mathrm{i}{\mathrm{O}}_2$(silica) and$\mathrm{T}\mathrm{i}{\mathrm{O}}_2:\mathrm{T}{\mathrm{a}}_2{\mathrm{O}}_5$(titania-doped tantala) and post-deposition annealing to 500°C to achieve low thermal noise and low optical absorption. Optical scattering by these coatings is a key limit to the sensitivity of the detectors. This paper describes optical scattering measurements for single-layer, ion-beam-sputtered thin films on fused silica substrates: two samples of$\mathrm{T}{\mathrm{a}}_2{\mathrm{O}}_5$and two of$\mathrm{T}\mathrm{i}{\mathrm{O}}_2:\mathrm{T}{\mathrm{a}}_2{\mathrm{O}}_5$. Using an imaging scatterometer at a fixed scattering angle of 12.8°, in-situ changes in the optical scatter of each sample were assessed during post-deposition annealing to 500°C in vacuum. The scatter of three of the four coated optics was observed to decrease during the annealing process, by 25–30% for tantala and up to 74% for titania-doped tantala, while the scatter from the fourth sample held constant. Angle-resolved scatter measurements performed before and after vacuum annealing suggest some improvement in three of the four samples. These results demonstrate that post-deposition, high-temperature annealing of single-layer tantala and titania-doped tantala thin films in vacuum does not lead to an increase in scatter, and may actually improve their scatter.