Imaging scatterometer for observing in situ changes to optical coatings during air annealing
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 mechanisms in situ and in real time during annealing. We present results that demonstrate in situ observation 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.
more »
« less
- PAR ID:
- 10426215
- Date Published:
- Journal Name:
- Applied Optics
- Volume:
- 62
- Issue:
- 7
- ISSN:
- 1559-128X
- Page Range / eLocation ID:
- B97
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
More Like this
-
High-quality optical coatings with low mechanical and optical losses are essential for the sensitivity of gravitational-wave detectors. While annealing is required to reduce the mechanical loss of amorphous coating materials, it often induces crystallization, which degrades optical performance through increased scattering. Standard characterization techniques, such as X-ray diffraction, are limited in detecting sparse populations of crystallites or characterizing their individual size distributions. In this work, we demonstrate a supplementary method based on angle-resolved Rayleigh–Mie scattering to detect and characterize individual crystallites within an amorphous coating. We apply this technique to a titanium-doped germania (GeO2:TiO2) coating, a promising material for future detectors, subjected to stepwise annealing at 625∘C. By comparing measured differential scattering cross-sections to T-matrix simulations, we extract the radius of individual defects and successfully monitor the evolution of the emerging defect population as a function of annealing. This technique allows for the detection of crystallites or other defects with radii down to ≈80nm and provides a complementary tool for studying the early stages of crystallization in low-noise optical coatings.more » « less
-
Abstract Titania doped with tantala is the high index material (high n) for the optical coatings used in LIGO and Virgo and its thermal noise limits LIGO/Virgo observations of astrophysical sources. In this paper, we study temperature induced changes to optical scatter of a multilayer highly reflective coating comprised of silica (low n) and titania doped with germania (high n) as a potential candidate to reduce coating thermal noise in ground-based observatories operating at room temperature. We observe that the scatter measured at 8° in a small region is low, with a median starting Bidirectional Reflectance Distribution Function (BRDF) of 1.1 × 10−7str−1increasing to 1.2 × 10−6str−1through annealing. The results presented here show the potential of adopting titania doped with germania coatings for future upgrades to LIGO and Virgo and as a pathfinder coating for Cosmic Explorer, a next-generation detector.more » « less
-
Abstract We report on the development and extensive characterization of co-sputtered tantala–zirconia (Ta 2 O 5 -ZrO 2 ) thin films, with the goal to decrease coating Brownian noise in present and future gravitational-wave detectors. We tested a variety of sputtering processes of different energies and deposition rates, and we considered the effect of different values of cation ratio η = Zr/(Zr + Ta) and of post-deposition heat treatment temperature T a on the optical and mechanical properties of the films. Co-sputtered zirconia proved to be an efficient way to frustrate crystallization in tantala thin films, allowing for a substantial increase of the maximum annealing temperature and hence for a decrease of coating mechanical loss φ c . The lowest average coating loss was observed for an ion-beam sputtered sample with η = 0.485 ± 0.004 annealed at 800 °C, yielding φ ¯ c = 1.8 × 1 0 − 4 rad. All coating samples showed cracks after annealing. Although in principle our measurements are sensitive to such defects, we found no evidence that our results were affected. The issue could be solved, at least for ion-beam sputtered coatings, by decreasing heating and cooling rates down to 7 °C h −1 . While we observed as little optical absorption as in the coatings of current gravitational-wave interferometers (0.5 parts per million), further development will be needed to decrease light scattering and avoid the formation of defects upon annealing.more » « less
-
The conformal nanoporous inorganic coatings with accessible pores that are stable under applied thermal and mechanical stresses represent an important class of materials used in the design of sensors, optical coatings, and biomedical systems. Here, we synthesize porous AlOx and ZnO coatings by the sequential infiltration synthesis (SIS) of two types of polymers that enable the design of porous conformal coatings—polymers of intrinsic microporosity (PIM) and block co-polymer (BCP) templates. Using quartz crystal microbalance (QCM), we show that alumina precursors infiltrate both polymer templates four times more efficiently than zinc oxide precursors. Using the quartz crystal microbalance (QCM) technique, we provide a comprehensive study on the room temperature accessibility to water and ethanol of pores in block copolymers (BCPs) and porous polymer templates using polystyrene-block-poly-4-vinyl pyridine (PS75-b-P4VP25) and polymers of intrinsic microporosity (PIM-1), polymer templates modified by swelling, and porous inorganic coatings such as AlOx and ZnO synthesized by SIS using such templates. Importantly, we demonstrate that no structural damage occurs in inorganic nanoporous AlOx and ZnO coatings synthesized via infiltration of the polymer templates during the water freezing/melting cycling tests, suggesting excellent mechanical stability of the coatings, even though the hardness of the inorganic nanoporous coating is affected by the polymer and precursor selections. We show that the hardness of the coatings is further improved by their annealing at 900 °C for 1 h, though for all the cases except ZnO obtained using the BCP template, this annealing has a negligible effect on the porosity of the material, as is confirmed by the consistency in the optical characteristics. These findings unravel new potential for the materials being used across various environment and temperature conditions.more » « less
An official website of the United States government

