A new deposition method developed by Goddard Space Flight Center fluorinates Al mirrors with XeF2 followed by a LiF coating to create what they term Al+XeLiF. This in-situ, room temperature process produces mirrors with high reflectivity in a broad spectral range, from the FUV to the IR, and is reported to be stable in relative humidities of 30% and lower. These mirrors are envisioned for missions requiring sensitivity down to 100 nm wavelength such as the habitable worlds observatory. Because most mission integration and testing campaigns require prolonged exposure to lab environments, and launch sites experience high relative humidities (RH) on average, some at 80% RH. We investigate Al+XeLiF stability in a wider range of temperatures and humidities along with employing additional characterization techniques including atomic force microscopy and x-ray photoelectron spectroscopy. We found that Al+XeLiF is stable in environments up to 82%RH when kept at cooler temperatures (3°C and 21°C). However, this material is unstable when stored at 60°C, experiencing roughening and loss in reflection from resulting Al surface plasmon excitation.
Astronomical instrumentation for measurements in the Far Ultraviolet (FUV, 90−200 nm) have historically considered aluminum (Al) thin film mirrors due to this material high reflectance over this wavelength range. However, the native aluminum oxide layer that forms on Al upon exposure to the atmosphere is strongly absorbing in this wavelength range, requiring that the films be protected with a dielectric that inhibits oxidation. Typically, magnesium fluoride (MgF2) or lithium fluoride (LiF) coatings are used as protective layers, but each has shortcomings. For example, MgF2 has an absorption cutoff at 115 nm that reduces performance below this wavelength, which is a critical part of the FUV spectrum for observational astrophysics. The use of LiF as a protection for Al provides a lower absorption cutoff at 100 nm, but it is hygroscopic and thus susceptible to degradation in humid conditions. Our team at GSFC has developed a new reactive Physical Vapor Deposition (rPVD) process that consists of a fluorination process with XeF2 gas combined with our traditional PVD process. We have found that this new rPVD process produces Al+XeF2+LiF (XeLiF) and Al+XeF2+MgF2 (XeMgF2) mirror coatings with unprecedented reflectance. In addition, the rPVD process seems to produce much more environmentally stable coatings (when compared to the conventional process without the XeF2 fluorination). We report on IR/Vis/UV reflectance of XeLiF and XeMgF2 mirrors. The surface roughness as well as the FUV reflectance measured over a period of 8 months for a XeLiF sample with a relatively thin (≃ 30 nm) Al layer are also reported. We have also been investigating the compatibility of this rPVD coating process for potential efficiency enhancements of Si-based gratings. Since it is known that the XeF2 vapor is a strong Si etchant, we are investigating if the native SiO2 layer on Si is sufficient to protect the groove profile of E-beam-ruled Si gratings from degradation. Preliminary results indicate that the native SiO2 layer is an effective barrier against etching of Si by XeF2.
Tabletop extreme ultraviolet (EUV) sources based on high harmonic generation (HHG) have been used as a powerful tool for probing magnetism. Obtaining magnetic information via magneto-optical contrast often requires the energy of the light to be tuned to magnetic resonance energies of the magnetic element present in the material; therefore, it is essential to calibrate the HHG spectrum to well defined absorption energies of materials. We have designed and assembled a HHG based EUV source for studying transition metal magnetic materials at their resonant M-absorption edges (35-75 eV of photon energy). One material of interest is iron, for which the iron M2,3 edge is 52.7 eV (23.5 nm wavelength) according to CXRO. We prepared and characterized a thin sample of iron for absorption spectroscopy and calibration of the absorption edge with beamline 6.3.2 at the Advance Light Source (ALS) in Lawrence Berkeley National Laboratory. This well characterized sample was capped with gold to prevent oxidation. From these measurements we extracted the absorption part of the index of refraction β spectrally and confirmed that the absorption edge of iron is 52.7 eV. With this information, we can better calibrate the HHG spectrum of our tabletop EUV source. Calibration of the HHG spectrum was achieved using model fitting the HHG spectrum using the grating equation and law of cosines while taking account into the results of the ALS data. We have determined that driving wavelength of the HHG process to be 773 nm. We also conclude that the chirp of the driving laser pulse can cause an energy shift to a HHG spectrum.
Aluminum mirrors protected by metal fluoride overcoats are crucial for FUV observations. Many contemplated missions specify optics elements with high reflectance down to 103 nm (Lyman beta). Lithium fluoride (LiF) has the highest band gap of any solid material and thus finds applications in FUV optics. However, LiF is difficult to work with because of its hygroscopic nature. The instability of these films was investigated by evaporating LiF onto silicon wafers and aging in environments with different relative humidities and temperatures. Samples were characterized using variable-angle spectroscopic ellipsometry (VASE) and atomic force microscopy (AFM). From these methods we found that storing LiF in a hot environment improved sample surface stability, and that in dry, hot environments, surfaces became more smooth after many hours in storage.
Lithium fluoride (LiF) is difficult to work with because of its hygroscopic nature (it pulls water out of air). The stability limits of LiF thin films and the nature of their failure when exposed to humid air are poorly understood. We show that LiF films undergo irreversible changes in optical properties and microstructure as determined by ellipsometry and SEM when exposed to dew points greater than 6 C. On the other hand, samples stored at a dew point of -22 C (4% RH at room temperature), showed only small changes in ellipsometric parameters. The ones stored at intermediate humidity 6 C (21% RH at room temperature) showed larger changes in ellipsometric parameters. SEM shows that deliquescence as well as efflorescence is important in LiF thin films. In situ spectroscopic ellipsometric measurements using a controlled variable humidity environment illuminates the changes in LiF thin films moving from moisture absorption to complete deliquescence.
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