Post-production correction of lamellar x-ray gratings by ion beam figuring
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Engineering topics
Publications and source records attributed to Gullikson, Eric M..
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We developed a new method of making ultra-low blaze angle diffraction gratings for x-ray applications. The method is based on reduction of the blaze angle of a master grating by nanoimprint replication followed by a plasma etch. A master blazed grating with a relatively large blaze angle is fabricated by anisotropic wet etching of a Si single crystal substrate. The surface of the master grating is replicated by a polymer material on top of a quartz substrate by nanoimprinting. Then a second nanoimprinting is performed using the 1st replica as a mold to replicate the saw-tooth surface into a resist layer on top of a Si grating substrate. A reactive ion etch is used to transfer the grating grooves into the Si substrate. The plasma etch provides reduction of the groove depth by a factor defined by the ratio of the etch rates for the resist and Si. We demonstrate reduction of the blaze angle of a master grating by a factor of 5 during fabrication of a 200 lines/mm blazed grating with a blaze angle of 0.2°. We investigated the quality and performance of the fabricated low blaze angle gratings and evaluate process accuracy and reproducibility. The new blaze angle reduction method preserves the planarity of the optical surface of the grating substrate and at the same time provides improvement in the grating groove quality during the reduction process.
We suggest a new method of making ultra-low blaze angle gratings for synchrotron application. The method is based on reduction of the blaze angle of a master grating by replication followed by a plasma etch. A master blazed grating with a relatively large blaze angle is fabricated by anisotropic wet etching of a Si single crystal substrate. The surface of the master grating is replicated by a polymer material on top of a quartz substrate by nanoimprinting and then transferred into quartz by a plasma etch. Then a 2nd nanoimprint step is applied to transfer the saw-tooth surface into a resist layer on top of a Si grating substrate. The plasma etch through the patterned resist layer provides transfer of the grooves into the Si substrate and results in reduction of the blaze angle due to the difference in etch rates of the resist and Si. We investigated the impact of the replication process on the groove shape, facet surface roughness, and diffraction efficiency of the fabricated 200 lines/mm low blaze angle grating.
Arcus is a proposed Explorer Class soft X-ray grating spectrometer. It aims to explore cosmic feedback by mapping hot gases within and between galaxies and galaxy clusters and characterizing jets and winds from supermassive black holes and to investigate the dynamics of protoplanetary disks and stellar accretion. Arcus features 12 m focal-length grazing-incidence silicon pore optics (SPO) developed for the Athena mission. Critical-angle transmission (CAT) gratings efficiently disperse high diffraction orders onto CCDs. We report new and improved X-ray performance results for Arcus-like CAT gratings, including a record resolving power for two coaligned CAT gratings. Multiple Arcus prototype grating facets were illuminated by an SPO at the PANTER facility. The facets consist of 32 × 32.5 mm 2 patterned silicon membranes, bonded to metal frames. The bonding angle is adjusted according to the measured average tilt angle of the grating bars in the membrane. Two simultaneously illuminated facets show a minor broadening of the Al-K α doublet in the 18th and 21st orders with the best-fit record effective resolving power of ${R}_{G}\approx {1.3}_{-0.5}^{+\infty }\times {10}^{4}$ (3σ), about three to four times the Arcus requirement. We measured the diffraction efficiency of quasi-fully illuminated gratings at O-K wavelengths in orders 4–7 in an Arcus-like configuration and compare results with synchrotron spot measurements. After corrections for geometrical effects and bremsstrahlung continuum, we find agreement between full and spot illumination at the two different facilities, as well as with the models used for Arcus effective area predictions. We find that these flight-like gratings meet the diffraction efficiency and greatly exceed the resolving power Arcus requires.
Standing wave ambient pressure photoemission spectroscopy (SWAPPS) is a promising method to investigate chemical and potential gradients across solid-vapor and solid-liquid interfaces under close-to-realistic environmental conditions, far away from high vacuum. Until now, these investigations have been performed only near room temperature, but for a wide range of interfacial processes, chief among them being heterogeneous catalysis, measurements at elevated temperatures are required. One concern in these investigations is the temperature stability of the multilayer mirrors, which generate the standing wave field. At elevated temperatures, degradation of the multilayer mirror due to, for example, interdiffusion between the adjacent layers, decreases the modulation of the standing wave field, thus rendering SWAPPS experiments much harder to perform. Here, we show that multilayer mirrors consisting of alternate B4C and W layers are stable at temperatures exceeding 600 °C and are, thus, promising candidates for future studies of surface and subsurface species in heterogeneous catalytic reactions using SWAPPS.
This manuscript presents the structural characterization of Al/Sc-based periodic multilayer coatings for the extreme ultraviolet (EUV) spectral range. Based on transmission electron microscopy and electron diffraction as well as grazing-incidence and large-angle x-ray diffraction, a model for the layer structure and the interfacial effects of Al/Sc coatings is built. The onset of crystallization in nanoscale Al and Sc layers as a function of thickness is also revealed in these characterizations. The Al/Sc layer model is validated and further refined by fitting in-band and out-of-band EUV reflectance measurements across 5 orders of magnitude in an extended wavelength range from 17 to 80 nm. Here, the same type of EUV reflectance measurements is used to test the Al/Sc aging properties and to demonstrate the spectral response of optimized two- and tri-material multilayers including Al/Sc, Al/Sc/SiC and Mo/Al/Sc.
The complex-valued index of refraction of germanium in the extreme ultraviolet (XUV) is measured by multiangle reflectance of synchrotron radiation. The resulting index of refraction is higher resolution than previously measured values. It reveals new structures attributed to transitions from the 3d-core orbitals to the $Σ^{c}_{5,2}$ and the $X^{c}_{5,2}$ conduction bands. Additionally, it is shown that the problem of total external reflection, which renders multi-angle reflectance measurements insensitive to the complex-valued refractive index at grazing incidence, can be overcome by employing measurements at angles of incidence away from the critical angle.
We introduce an experimental, self-consistent determination of the optical constants (refractive index) of Pt using a combination of photoabsorption and reflectance data in the photon energy range 25–778 eV, which includes the N- and O-shell electronic absorption edges of Pt. We compare our new experimental values with Pt optical constant data sets from the literature. Our Pt optical constant values demonstrate highly resolved absorption-edge fine structure around the O 2,3 and N 6,7 edges in both the absorptive and dispersive portions of the refractive index, which were missing in the earlier literature.
Extreme ultraviolet (XUV) transient reflectivity around the germanium M 4,5 edge (3d core-level to valence transition) at 30 eV is advanced to obtain the transient dielectric function of crystalline germanium [100] on femtosecond to picosecond time scales following photoexcitation by broadband visible-to-infrared (VIS/NIR) pulses. By fitting the transient dielectric function, carrier-phonon induced relaxations are extracted for the excited carrier distribution. The measurements reveal a hot electron relaxation rate of 3.2±0.2ps attributed to the X-L intervalley scattering and a hot hole relaxation rate of 600±300fs ascribed to intravalley scattering within the heavy hole (HH) band, both in good agreement with previous work. An overall energy shift of the XUV dielectric function is assigned to a thermally induced band gap shrinkage by formation of acoustic phonons, which is observed to be on a timescale of 4-5 ps, in agreement with previously measured optical phonon lifetimes. The results reveal that the transient reflectivity signal at an angle of 66° with respect to the surface normal is dominated by changes to the real part of the dielectric function, due to the near critical angle of incidence of the experiment (66°-70° for the range of XUV energies used. Finally, this work provides a methodology for interpreting XUV transient reflectivity near core-level transitions, and it demonstrates the power of the XUV spectral region for measuring ultrafast excitation dynamics in solids.
It is well established that extreme ultraviolet (EUV) mask multilayer roughness leads to wafer-plane linewidth roughness (LWR) in the lithography process. Analysis and modeling done to date has assumed, however, that the roughness leading to scatter is primarily a phase effect and that the amplitude can be ignored. Under this assumption, simple scattering measurements can be used to characterize the statistical properties of the mask roughness. Here, we explore the implications of this simplifying assumption by modeling the imaging impacts of the roughness amplitude component as a function of the balance between amplitude and phase induced scatter. In addition to model-based analysis, we also use an EUV microscope to compare experimental through focus data to modeling in order to assess the actual amount of amplitude roughness on a typical EUV multilayer mask. The results indicate that amplitude roughness accounts for less than 1% of the total scatter for typical EUV masks.
Efficiently detecting the B-K emission band around 6.76 nm from a trace concentration of boron in steel compounds has motivated a theoretical exploration of means of increasing the diffraction efficiency of a laminar grating with carbon overcoating. To experimentally evaluate this enhancement, a Ni grating was coated with a high-density carbon film, i.e., diamond-like carbon (DLC). The first order diffraction efficiencies of the Ni gratings coated with and without DLC were measured to be 25.8 % and 16.9 %, respectively, at a wavelength of 6.76 nm and an angle of incidence of 87.07°. The ratio of diffraction efficiency obtained experimentally vs. that calculated by numerical simulation is 0.87 for the DLC-coated Ni grating. The diffraction efficiency of a Ni grating coated with a low-density carbon film, amorphous carbon (a-C), was also slightly improved to be 19.6 %. Furthermore, a distinct minimum of the zeroth order lights of the two carbon-coated Ni gratings were observed at around 6.76 nm, which is coincident with the maximum of the first order light.
Diffraction gratings are used from micron to nanometer wavelengths as dispersing elements in optical instruments. At shorter wavelengths, crystals can be used as diffracting elements, but due to the 3D nature of the interaction with light are wavelength selective rather than wavelength dispersing. There is an urgent need to extend grating technology into the x-ray domain of wavelengths from 1 to 0.1 nm, but this requires the use of gratings that have a faceted surface in which the facet angles are very small, typically less than 1°. Small facet angles are also required in the extreme ultra-violet and soft x-ray energy ranges in free electron laser applications, in order to reduce power density below a critical damage threshold. In this work, we demonstrate a technique based on anisotropic etching of silicon designed to produce very small angle facets with a high degree of perfection.
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Recent advances in the development of attosecond soft X-ray sources ranging into the water window spectral range, between the 1s states of carbon and oxygen (284 eV–543 eV), are also driving the development of suited broadband multilayer optics for steering and shaping attosecond pulses. The relatively low intensity of current High Harmonic Generation (HHG) soft X-ray sources calls for an efficient use of photons, thus the development of low-loss multilayer optics is of uttermost importance. Here, we report about the realization of broadband Cr/Sc attosecond multilayer mirrors with nearly atomically smooth interfaces by an optimized ion beam deposition and assisted interface polishing process. This yields to our knowledge highest multilayer mirror reflectivity at 300 eV near normal incidence. The results are verified by transmission electron microscopy (TEM) and soft/hard X-ray reflectometry.
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Explore the source record for details and available documents.
Explore the source record for details and available documents.