We report on the use of multilayer Laue lenses to focus the intense X-ray Free Electron Laser (XFEL) beam at the European XFEL to a spot size of a few tens of nanometers. We present the procedure to align and characterize these lenses and discuss challenges working with the pulse trains from this unique x-ray source.
We report on the fabrication of novel diffraction gratings for soft x-ray and extreme ultra-violet (EUV) photon energies based on asymmetric-cut multilayer structures. Asymmetric-cut multilayers are highly dispersive and highly efficient gratings obtained by slicing a thick multilayer coating. Multilayer deposition techniques enable sub-ångström precision in layer thickness control, which leads to close to perfect blazed gratings. However, the final grating size is limited by the maximum multilayer thickness for which one can still control the layer thickness, stress and roughness. Here, we present a new approach in which we substantially extend the grating size by combining specially prepared substrates, thick multilayer deposition and final polishing. Gratings prepared by this method, like asymmetric multilayers deposited on plane substrates, are highly dispersive and efficient. Their extended size make them ideal for use in monochromators, spectrometers and pulse compressors.
Adam F. Leontowich, Andrew Aquila, Francesco Stellato, Richard Bean, Holger Fleckenstein, Mauro Prasciolu, Mengning Liang, Daniel DePonte, Anton Barty, Fenglin Wang, Jakob Andreasson, Janos Hajdu, Henry Chapman, Saša Bajt
A super-polished substrate with an off-axis parabola figure was coated with a Sc/B4C/Cr multilayer. This optic was used to focus pulses of 4.3 nm photons from the Free-electron LASer in Hamburg (FLASH) at normal incidence. Beam imprints were made in poly(methyl methacrylate) to align the optic and to measure the beam profile at the focal plane. The intense interaction resulted in imprints with raised perimeters, surrounded by ablated material extending out several micrometres. These features interfere with the beam profile measurement. The effect of a post-exposure development step on the beam imprints was investigated.
N. Loh, Dmitri Starodub, Lukas Lomb, Christina Hampton, Andrew Martin, Raymond Sierra, Anton Barty, Andrew Aquila, Joachim Schulz, Jan Steinbrener, Robert Shoeman, Stephan Kassemeyer, Christoph Bostedt, John Bozek, Sascha Epp, Benjamin Erk, Robert Hartmann, Daniel Rolles, Artem Rudenko, Benedikt Rudek, Lutz Foucar, Nils Kimmel, Georg Weidenspointner, Günther Hauser, Peter Holl, Emanuele Pedersoli, MengNing Liang, Mark Hunter, Lars Gumprecht, Nicola Coppola, Cornelia Wunderer, Heinz Graafsman, Filipe R. N. Maia, Tomas Ekeberg, Max Hantke, Holger Fleckenstein, Helmut Hirsemann, Karol Nass, Thomas White, Herbert Tobias, George Farquar, W. Henry Benner, Stefan Hau-Riege, Christian Reich, Andreas Hartmann, Heike Soltau, Stefano Marchesini, Sasa Bajt, Miriam Barthelmess, Lothar Strueder, Joachim Ullrich, Philip Bucksbaum, Keith Hodgson, Mathias Frank, Ilme Schlichting, Henry Chapman, Michael Bogan
Profiling structured beams produced by X-ray free-electron lasers (FELs) is crucial to both maximizing signal intensity for weakly scattering targets and interpreting their scattering patterns. Earlier ablative imprint studies describe how to infer the X-ray beam profile from the damage that an attenuated beam inflicts on a substrate. However, the beams in-situ profile is not directly accessible with imprint studies because the damage profile could be different from the actual beam profile. On the other hand, although a Shack-Hartmann sensor is capable of in-situ profiling, its lenses may be quickly damaged at the intense focus of hard X-ray FEL beams. We describe a new approach that probes the in-situ morphology of the intense FEL focus. By studying the translations in diffraction patterns from an ensemble of randomly injected sub-micron latex spheres, we were able to determine the non-Gaussian nature of the intense FEL beam at the Linac Coherent Light Source (SLAC National Laboratory) near the FEL focus. We discuss an experimental application of such a beam-profiling technique, and the limitations we need to overcome before it can be widely applied.
The development of plasma excited X-ray lasers is of interest for many scientific applications. The photon energies and
peak brilliance of these lasers sources are well suited for probing atomic, molecular and solid state systems. The
development and improvement in these laser systems also drives a need for metrologies of the properties of these lasers.
Our research implements X-ray optics, designed to operate at the Brewster's angle, to measure the polarization state of a
Ni-like Sn laser. The device determines the polarization state on a shot to shot basis and opens the possibility for
polarization control of plasma excited X-ray lasers and thus probing spin polarized electronic states.
Andrew Martin, Jakob Andreasson, Andrew Aquila, Saša Bajt, Thomas R. Barends, Miriam Barthelmess, Anton Barty, W. Henry Benner, Christoph Bostedt, John Bozek, Phillip Bucksbaum, Carl Caleman, Nicola Coppola, Daniel DePonte, Tomas Ekeberg, Sascha Epp, Benjamin Erk, George Farquar, Holger Fleckenstein, Lutz Foucar, Matthias Frank, Lars Gumprecht, Christina Hampton, Max Hantke, Andreas Hartmann, Elisabeth Hartmann, Robert Hartmann, Stephan Hau-Riege, Günther Hauser, Peter Holl, André Hoemke, Olof Jönsson, Stephan Kassemeyer, Nils Kimmel, Maya Kiskinova, Faton Krasniqi, Jacek Krzywinski, Mengning Liang, Ne-Te Duane Loh, Lukas Lomb, Filipe R. N. Maia, Stefano Marchesini, Marc Messerschmidt, Karol Nass, Duško Odic, Emanuele Pedersoli, Christian Reich, Daniel Rolles, Benedikt Rudek, Artem Rudenko, Carlo Schmidt, Joachim Schultz, M. Marvin Seibert, Robert Shoeman, Raymond Sierra, Heike Soltau, Dmitri Starodub, Jan Steinbrener, Francesco Stellato, Lothar Strüder, Martin Svenda, Herbert Tobias, Joachim Ullrich, Georg Weidenspointner, Daniel Westphal, Thomas White, Garth Williams, Janos Hajdu, Ilme Schlichting, Michael Bogan, Henry Chapman
Results of coherent diffractive imaging experiments performed with soft X-rays (1-2 keV) at the Linac Coherent
Light Source are presented. Both organic and inorganic nano-sized objects were injected into the XFEL beam
as an aerosol focused with an aerodynamic lens. The high intensity and femtosecond duration of X-ray pulses
produced by the Linac Coherent Light Source allow structural information to be recorded by X-ray diffraction
before the particle is destroyed. Images were formed by using iterative methods to phase single shot diffraction
patterns. Strategies for improving the reconstruction methods have been developed. This technique opens
up exciting opportunities for biological imaging, allowing structure determination without freezing, staining or
crystallization.
The recent commissioning of a X-ray free-electron laser triggered an extensive research in the area of X-ray ablation of
high-Z, high-density materials. Such compounds should be used to shorten an effective attenuation length for obtaining
clean ablation imprints required for the focused beam analysis. Compounds of lead (Z=82) represent the materials of first
choice. In this contribution, single-shot ablation thresholds are reported for PbWO4 and PbI2 exposed to ultra-short
pulses of extreme ultraviolet radiation and X-rays at FLASH and LCLS facilities, respectively. Interestingly, the
threshold reaches only 0.11 mJ/cm2 at 1.55 nm in lead tungstate although a value of 0.4 J/cm2 is expected according to
the wavelength dependence of an attenuation length and the threshold value determined in the XUV spectral region, i.e.,
79 mJ/cm2 at a FEL wavelength of 13.5 nm. Mechanisms of ablation processes are discussed to explain this discrepancy.
Lead iodide shows at 1.55 nm significantly lower ablation threshold than tungstate although an attenuation length of the
radiation is in both materials quite the same. Lower thermal and radiation stability of PbI2 is responsible for this finding.
Temperature stability of Mo/B4C multilayers with normal incidence peak reflectivity at 7 nm was investigated in a
temperature range between 100°C and 900°C. With this multilayer pair we achieved up to 24% reflectivity in the asdeposited
state at 6.7 nm. We investigated the effect of post-deposition annealing temperature and time on intrinsic
stress, period and normal incidence reflectivity. We observed that stress alters almost linearly with temperature up to
600°C. In this temperature range the multilayer period expands by <1%. The major change in stress and period occurs in
the first minutes of heat treatment. The stress relaxation is accompanied with volume and packing density increase
(period expansion). This process, which happens within minutes, is followed by a diffusion controlled process.
We report on the x-ray absorption of Warm Dense Matter experiment at the FLASH Free Electron Laser (FEL) facility at DESY. The FEL beam is used to produce Warm Dense Matter with soft x-ray absorption as the probe of electronic structure. A multilayer-coated parabolic mirror focuses the FEL radiation, to spot sizes as small as 0.3μm in a ~15fs pulse of containing >1012 photons at 13.5 nm wavelength, onto a thin sample. Silicon photodiodes measure the transmitted and reflected beams, while spectroscopy provides detailed measurement of the temperature of the sample. The goal is to measure over a range of intensities approaching 1018 W/cm2. Experimental results will be presented along with theoretical calculations. A brief report on future FEL efforts will be given.
The beam of Free-Electron Laser in Hamburg (FLASH) tuned at either 32.5 nm or 13.7 nm was focused by a grazing
incidence elliptical mirror and an off-axis parabolic mirror coated by Si/Mo multilayer on 20-micron and 1-micron spot,
respectively. The grazing incidence and normal incidence focusing of ~10-fs pulses carrying an energy of 10 μJ lead at
the surface of various solids (Si, Al, Ti, Ta, Si3N4, BN, a-C/Si, Ni/Si, Cr/Si, Rh/Si, Ce:YAG, poly(methyl methacrylate)
- PMMA, stainless steel, etc.) to an irradiance of 1013 W/cm2 and 1016 W/cm2, respectively. The optical emission of the
plasmas produced under these conditions was registered by grating (1200 lines/mm and/or 150 lines/mm) spectrometer
MS257 (Oriel) equipped with iCCD head (iStar 720, Andor). Surprisingly, only lines belonging to the neutral atoms
were observed at intensities around 1013 W/cm2. No lines of atomic ions have been identified in UV-vis spectra emitted
from the plasmas formed by the FLASH beam focused in a 20-micron spot. At intensities around 1016 W/cm2, the OE
spectra are again dominated by the atomic lines. However, a weak emission of Al+ and Al2+ was registered as well. The
abundance ratio of Al/Al+ should be at least 100. The plasma is really cold, an excitation temperature equivalent to 0.8 eV was found by a computer simulation of the aluminum plasma OE spectrum. A broadband emission was also
registered, both from the plasmas (typical is for carbon; there were no spectral lines) and the scintillators (on Ce:YAG
crystal, both the luminescence bands and the line plasma emission were recorded by the spectrometer).
A multilayer-coated 27-cm focal length parabola, optimized to reflect 13.5 nm wavelength at normal incidence,
was used in multiple FLASH experiments and focused the beam to a sub-micron beam size. The intensity of the beam
was measured indirectly from the depths of craters left by the FLASH beam on PMMA-coated substrates. Comparing
simulated and experimental shapes of the craters we found the best match for a wavefront error of 0.45 nm, or λ/30. We
further estimated that the FWHM of the focal spot was 350 nm and that the intensity in the focus was 1018 W/cm2. The
sub-micron FLASH beam provided extreme intensity conditions essential for warm dense matter experiments. The same
optic was used in multiple experiments and survived the beam. However, after the first measurements, which took place
over several days, the optical surface was contaminated. This contamination reduced the mirror reflectivity, which was
partially recovered by oxygen plasma cleaning. However, even the partially cleaned multilayer-coated optic is still
diffraction limited and can focus the beam in future experiments to a sub-micron beam size.
One of the remaining challenges for the commercialization of EUV lithography is the lifetime of
the Mo/Si multilayer optics and masks. The lifetime is dominated by carbon contamination on the surfaces
of the optics, which is caused by residual hydrocarbons in the vacuum chamber when optics are exposed to
EUV radiation. One of the possible sources of the hydrocarbons in the chamber is resist outgassing. To be
able to understand which type of hydrocarbons are harmful to EUV mirror reflectivity, three hydrocarbon
species - benzene, tert-butanol and diphenyl sulfide - which are thought to be representative of commonly
outgassed species from EUV photoresist were selected. The goal of this work was to measure the
contamination rate from these three species and to be able to draw conclusions about other species. The
results of the experiments showed that after 8 hours of exposure there was not enough contamination to be
significantly measurable. In addition to these hydrocarbon species, we also used vacuum grease and carbon
tape as an outgassing source for hydrocarbons. Comparatively, high contamination rates were achieved
with vacuum grease and carbon tape.
Extreme ultraviolet (EUV) photoresists are known to outgas during exposure to EUV radiation in the vacuum
environment. This is of particular concern since some of the outgassed species may contaminate the nearby EUV optics
and cause a loss of reflectivity and therefore throughput of the EUV exposure tools. Due to this issue, work has been
performed to measure the species and quantities that outgas from EUV resists. Additionally, since the goal of these
measurements is to determine the relative safety of various resists near EUV optics, work has been performed to measure
the deposition rate of the outgassed molecules on Mo/Si-coated witness plate samples. The results for various species
and tests show little measurable effect from resist components on optics contamination with modest EUV exposure
doses.
Multilayers are artificially layered structures that can be used to create optics and optical elements for a broad
range of x-ray wavelengths, or can be optimized for other applications. The development of next generation x-ray
sources (high brightness synchrotrons and x-ray free electron lasers) requires advances in x-ray optics. Newly
developed multilayer-based mirrors and optical elements enabled efficient band-pass filtering, focusing and time
resolved measurements in recent FLASH (Free Electron LASer in Hamburg) experiments. These experiments are
providing invaluable feedback on the response of the multilayer structures to high intensity, short pulsed x-ray sources.
This information is crucial to design optics for future x-ray free electron lasers and to benchmark computer codes that
simulate damage processes.
Endurance testing of Ru-capped multilayer mirrors (MLMs) at the NIST synchrotron facility has revealed that the damage resulting from EUV irradiation in a water-dominated environment is nonlinear and may be influenced by competing oxidation and carbon-deposition processes. Concurrent results from two different environmental chambers reveal non-intuitive relationships between reflectivity loss and the admitted water-vapor partial pressure, the ambient background-gas composition, the presence or absence of hot filaments in the chamber, the EUV intensity and the irradiation dose. We discuss possible mechanisms and propose further experiments to test them. Determining the MLM lifetime from accelerated tests is a very difficult task. It is crucial that any lifetime testing procedure involves duplicate exposures for consistency, and, if possible, testing in multiple facilities.
The oxidation resistance of protective capping layers for extreme ultraviolet lithography (EUVL) multilayers depends on their microstructure. Differently prepared Ru-capping layers, deposited on Mo/Si EUVL multilayers, are investigated to establish their baseline structural, optical, and surface properties in an as-deposited state. The same capping layer structures are then tested for their thermal stability and oxidation resistance. The best performing Ru-capping layer structure is analyzed in detail with transmission electron microscopy (TEM). Compared to other Ru-capping layer preparations studied here, it is the only one that shows grains with preferential orientation. This information is essential to model and optimize the performance of EUVL multilayers.
Recently, while performing extensive EUV irradiation endurance testing on Ru-capped multilayer mirrors in the presence of elevated partial pressures of water and hydrocarbons, NIST has observed that the amount of EUV-induced damage actually decreases with increasing levels of water vapor above ~5x10-7 Torr. It is thought that the admitted water vapor may interact with otherwise stable, condensed carbonaceous species in an UHV vacuum system to increase the background levels of simple gaseous carbon-containing molecules. Some support for this hypothesis was demonstrated by observing the mitigating effect of very small levels of simple hydrocarbons with the intentional introduction of methyl alcohol in addition to the water vapor. It was found that the damage rate decreased by at least an order of magnitude when the partial pressure of methyl alcohol was just one percent of the water partial pressure. These observations indicate that the hydrocarbon components of the vacuum environment under actual testing conditions must be characterized and controlled to 10-11 Torr or better in order to quantify the damage caused by high levels of water vapor. The possible effects of exposure beam size and out-of-band radiation on mirror lifetime testing will also be discussed.
Since 1993, research in the fabrication of extreme ultraviolet (EUV) optical imaging systems, conducted at Lawrence Berkeley National Laboratory (LBNL) and Lawrence Livermore National Laboratory (LLNL), has produced the highest resolution optical systems ever made. We have pioneered the development of ultra-high-accuracy optical testing and alignment methods, working at extreme ultraviolet wavelengths, and pushing wavefront-measuring interferometry into the 2-20-nm wavelength range (60-600 eV). These coherent measurement techniques, including lateral shearing interferometry and phase-shifting point-diffraction interferometry (PS/PDI) have achieved RMS wavefront measurement accuracies of 0.5-1-Å and better for primary aberration terms, enabling the creation of diffraction-limited EUV optics. The measurement accuracy is established using careful null-testing procedures, and has been verified repeatedly through high-resolution imaging. We believe these methods are broadly applicable to the advancement of short-wavelength optical systems including space telescopes, microscope objectives, projection lenses, synchrotron beamline optics, diffractive and holographic optics, and more. Measurements have been performed on a tunable undulator beamline at LBNL's Advanced Light Source (ALS), optimized for high coherent flux; although many of these techniques should be adaptable to alternative ultraviolet, EUV, and soft x-ray light sources. To date, we have measured nine prototype all-reflective EUV optical systems with NA values between 0.08 and 0.30 (f/6.25 to f/1.67). These projection-imaging lenses were created for the semiconductor industry's advanced research in EUV photolithography, a technology slated for introduction in 2009-13. This paper reviews the methods used and our program's accomplishments to date.
We are developing polymer smoothing processes on diamond-turned (metal) and ground (metal or ceramic) substrates to reduce high and mid-spatial frequency roughness, for implementation as EUVL condenser optics. Diamond-turning or grinding can be used as relatively inexpensive processes to obtain the specified optic figure, however, the resulting surface has high-spatial roughness in the order of tens or hundreds of Angstroms, which would prohibit normal incidence operation at EUV wavelengths due to extremely low reflectance. Our polymer smoothing process reduces roughness to a few Angstroms, thus enabling normal-incidence operation. The substrate material and smoothing film have to combine a unique set of properties such as chemical compatibility, high thermal stability and low stress to be able to operate inside alternative-fuel EUVL source environments. Experimental results are presented on the development, testing and performance of these novel substrates.
Differently prepared Ru-capping layers, deposited on Mo/Si EUV multilayers, have been characterized using a suite of metrologies to establish their baseline structural, optical, and surface properties in as-deposited state. The same capping layer structures were tested for their thermal stability and oxidation resistance. Post-mortem characterization identified changes due to accelerated tests. The best performing Ru-capping layer structure was studied in detail with transmission electron microscopy to identify the grain microstructure and texture. This information is essential for modeling and performance optimization of EUVL multilayers.
Zone plates with depth to zone-width ratios as large as 100 are needed for focusing of hard x-rays. Such high aspect ratios are challenging to produce by lithography. We are investigating the fabrication of high-aspect-ratio linear zone plates by multilayer deposition followed by sectioning. As an initial step in this work, we present a synchrotron x-ray study of constant-period multilayers diffracting in Laue (transmission) geometry. Data are presented from two samples: a 200 period W/Si multilayer with d-spacing of 29 nm, and a 2020 period Mo/Si multilayer with d-spacing of 7 nm. By cutting and polishing we have successfully produced thin cross sections with section depths ranging from 2 to 12 μm. Transverse scattering profiles (rocking curves) across the Bragg reflection exhibit well-defined interference fringes originating from the depth of the sample, in agreement with dynamical diffraction theory for a multilayer in Laue geometry.
We have produced and characterized Mo/Y multilayers designed as linear-polarizers for use near λ ~ 8 nm. By depositing these films directly onto silicon photodiodes, we are able to measure both reflectance and transmittance in the EUV using synchrotron radiation. These measurements have been used to access the accuracy of yttrium optical constants in this wavelength range. We describe our experimental results and discuss the prospects for the future development of efficient EUV polarization elements.
The design of Mo/Si and Mo/Y multilayers as EUV polarizers is presented. The polarization performance of these multilayers was calculated based on their optical properties at around Brewster angles. The polarization results of a silicon photodiode that was coated with an interface-engineered Mo/Si multilayer are described. The sensitivity of this specially-coated photodiode and its polarization responses were determined from both reflectance and transmittance of the multilayer coating, using synchrotron radiation. The multilayer reflected 69.8% of s-polarized light and only 2.4% of p-polarized light, therefore transmitted about 0.2% s-polarized light and 8.4% p-polarized light at 13.5 nm to the underlying photodiode substrate. A polarization ratio based on transmittance values, (Tp-Ts)/(Tp+Ts), of 95% was achieved with sufficiently high sensitivity. This result demonstrates the usefulness of Mo/Si multilayer-coated photodiodes as future EUV polarimeters.
We report on 2D near-field imaging experiments of the 11.9-nm Sn x-ray laser that were performed with a set of novel Mo/Y multilayer mirrors having reflectivities of up to 40% at normal and at 45° incidence. Second-moment analysis of the x-ray laser emission was used to determine values of the c-ray beam propagation factor M2 for a range of irradiation parameters. The results reveal a reduction of M2 with increasing prepulse intensity. The spatial size of the output is a factor of ~2 smaller than previously measured for the Pd x-ray laser, while the distance of the x-ray emission with respect to the target surface remains roughly the same.
Recent studies have been conducted to investigate the use of atomic hydrogen as an in-situ contamination removal method for EUV optics. In these experiments, a commercial source was used to produce atomic hydrogen by thermal dissociation of molecular hydrogen using a hot filament. Samples for these experiments consisted of silicon wafers coated with sputtered carbon, Mo/Si optics with EUV-induced carbon, and bare Si-capped and Ru-B4C-capped Mo/Si optics. Samples were exposed to an atomic hydrogen source at a distance of 200 - 500 mm downstream and angles between 0-90° with respect to the source. Carbon removal rates and optic oxidation rates were measured using Auger electron spectroscopy depth profiling. In addition, at-wavelength peak reflectance (13.4 nm) was measured using the EUV reflectometer at the Advanced Light Source. Data from these experiments show carbon removal rates up to 20 Å/hr for sputtered carbon and 40 Å/hr for EUV deposited carbon at a distance of 200 mm downstream. The cleaning rate was also observed to be a strong function of distance and angular position. Experiments have also shown that the carbon etch rate can be increased by a factor of 4 by channeling atomic hydrogen through quartz tubes in order to direct the atomic hydrogen to the optic surface. Atomic hydrogen exposures of bare optic samples show a small risk in reflectivity degradation after extended periods. Extended exposures (up to 20 hours) of bare Si-capped Mo/Si optics show a 1.2% loss (absolute) in reflectivity while the Ru-B4C-capped Mo/Si optics show a loss on the order of 0.5%. In order to investigate the source of this reflectivity degradation, optic samples were exposed to atomic deuterium and analyzed using low energy ion scattering direct recoil spectroscopy to determine any reactions of the hydrogen with the multilayer stack. Overall, the results show that the risk of over-etching with atomic hydrogen is much less than previous studies using RF discharge cleaning while providing cleaning rates suitable for EUV lithography operations.
The reflectance stability of multilayer coatings for extreme ultraviolet lithography (EUVL) in a commercial tool environment is of utmost importance to ensure continuous exposures with minimum maintenance cost. We have made substantial progress in designing the protective capping layer coatings, understanding their performance and estimating their lifetimes based on accelerated electron beam and EUV exposure studies. Our current capping layer coatings have about 40 times longer lifetimes than Si-capped multilayer optics. Nevertheless, the lifetime of current Ru-capped multilayers is too short to satisfy commercial tool requirements and further improvements are essential.
Extreme ultraviolet (EUV)-induced oxidation of silicon-capped, [Mo/Si] multilayer mirrors in the presence of background levels of water vapor is recognized as one of the most serious threats to multilayer lifetime since oxidation of the top silicon layer is an irreversible process. The current work directly compares the oxidation on a silicon-capped, [Mo/Si] multilayers caused by EUV photons with the oxidation caused by 1 keV electrons in the presence of the same water vapor environment (2 x 10-6 Torr). Similar, 4 nm, silicon-capped, [Mo/Si] multilayer mirror samples were exposed to photons (95.3 eV) + water vapor at the ALS, LBNL, and also to a 1 keV electron beam + water vapor in separate experimental systems. The results of this work showed that the oxidation produced by ~1 µA of e-beam current was found to be equivalent to that produced by ~1 mW of EUV exposure. These results will help allow the use of 1 keV electrons beams, instead of EUV photons, to perform environmental testing of multilayers in a low-pressure water environment and to more accurately determine projected mirror lifetimes based on the electron beam exposures.
Commercial EUV lithographic systems require multilayers with higher reflectance and better stability then that published to date. This work represents our effort to meet these specifications. Interface-engineered Mo/Si multilayers with 70% reflectance at 13.5 nm wavelength (peak width of 0.545 nm) and 71% at 12.7 nm wavelength (peak width of 0.49 nm) were developed. These results were achieved with 50 bilayers. These new multilayers consist of Mo and Si layers separated by thin boron carbide layers. Depositing boron carbide on interfaces leads to reduction in silicide formation of the Mo-on-Si interfaces. Bilayer contraction is reduced by 30% implying that there is less intermixing of Mo and Si to form silicide. As a result the Mo-on-Si interfaces are sharper in interface-engineered multilayers than in standard Mo/Si multilayers. The optimum boron carbide thicknesses have been determined and appear to be different for Mo-on-Si and Si-on-Mo interfaces. The best results were obtained with 0.4 nm thick boron carbide layer for the Mo-on-Si interface and 0.25 nm thick boron carbide layer for the Si-on-Mo interface. Increase in reflectance is consistent with multilayers with sharper and smoother interfaces. A significant improvement in oxidation resistance of EUV multilayers has been achieved with ruthenium terminated Mo/Si multilayers. The best capping layer design consists of a Ru layer separated from the last Si layer by a boron carbide diffusion barrier. This design achieves high reflectance and the best oxidation resistance in a water vapor (i.e. oxidation) environment. Electron beam exposures of 4.5 hours in the presence of 5x10-7 torr water vapor partial pressure show no measurable reflectance loss and no increase in the oxide thickness of Ru terminated multilayers. Longer exposures in different environments are necessary to test lifetime stability of many years.
With the acceptance of AAPSM’s by most major semiconductor manufacturers, it is necessary to build a significant number of these masks in a cost effective and controlled manner. Optical methods of metrology used for many years in the photomask industry for binary masks are unsuitable for certain metrology applications related to AAPSM manufacture and repair. Recent work performed on a Dimension 9000M-PM automated atomic force microscope shows promise for both process control and defect review applications for AAPSM’s and overcome some of the limitations of optical and SEM based metrologies. AFM metrology is shown to be able to quantify shifter step heights and phase error for features as small as 100 nm. Further, these systems are able to read in defect coordinate maps and automatically drive to these sites and scan. The scanned data provides pixel-by-pixel height data that can be used by repair tools to establish the proper dose for defect ablation.
Synchrotron-based reflectometry is an important technique for the precise determination of optical properties of reflective multilayer coatings for Extreme Ultraviolet Lithography (EUVL). Multilayer coatings enable normal incidence reflectances of more than 65% in the wavelength range between 11 and 15 nm. In order to achieve high resolution and throughput of EUVL systems, stringent requirements not only apply to their mechanical and optical layout, but also apply to the optical properties of the multilayer coatings. Therefore, multilayer deposition on near-normal incidence optical surfaces of projection optics, condenser optics and reflective masks requires suitable high-precision metrology. Most important, due to their small bandpass on the order of only 0.5 nm, all reflective multilayer coatings in EUVL systems must be wavelength-matched to within +/- 0.05 nm. In some cases, a gradient of the coating thickness is necessary for wavelength matching at variable average angle of incidence in different locations on the optical surfaces. Furthermore, in order to preserve the geometrical figure of the optical substrates, reflective multilayer coatings need to be uniform to within 0.01 nm in their center wavelength. This requirement can only be fulfilled with suitable metrology, which provides a precision of a fraction of this value. In addition, for the detailed understanding and the further development of reflective multilayer coatings a precision in the determination of peak reflectances is desirable on the order of 0.1%. Substrates up to 200 mm in diameter and 15 kg in mass need to be accommodated. Above requirements are fulfilled at beamline 6.3.2 of the Advanced Light Source (ALS) in Berkeley. This beamline proved to be precise within 0.2% (rms) for reflectance and 0.002 nm (rms) for wavelength.
Extreme Ultra-Violet lithography is one of the leading next generation lithography options. Currently, EUV masks are routinely made of reflective mirrors made of Mo/Si multi- layers, which have a peak reflectivity of 67.5% at a wavelength of 13.4 nm. However, in order to increase the throughput of an EUVL system, a new set of Be-based multi- layers are being developed, which have a peak reflectivity of near 70% at 11.4. The two materials that have recently been developed are Mo/Be and MoRu/Be multi-layers. Beryllium based multi-layer masks show great promise for a significant increase in the lithography system throughput (2 - 3X over the current Mo/Si multi-layer mask) due to their increased reflectivity and bandwidth at 11.4 nm where the xenon laser plasma source is more intense. We have successfully developed a process to fabricate masks using Be-based multi-layers. The absorber stack consists of TaSiN (absorber), SiON (repair buffer) and Cr (conductive etch stop) deposited on the multi- layer mirror. Lawrence Livermore National Laboratory supplied the Mo/Be and MoRu/Be multi-layer mirrors used to fabricate the masks. Completed masks were exposed at Sandia National Laboratories' 10X EUV exposure system and equal lines and spaces down to 80 nm were successfully printed. The paper addresses the issues and challenges to fabricate the mask using Be-based multi-layers and a comparison will be made with the Mo/Si multi-layer mask patterning process.
Extreme Ultraviolet Lithography (EUVL) is a candidate for future application by the semiconductor industry in the production of sub-100 nm feature sizes in integrated circuits. Using multilayer reflective coatings optimized at wavelengths ranging from 11 to 14 nm, EUVL represents a potential successor to currently existing optical lithography techniques. In order to assess lifetimes of the multilayer coatings under realistic conditions, a series of radiation stability tests has been performed. In each run a dose of EUV radiation equivalent to several months of lithographic operation was applied to Mo/Si and Mo/Be multilayer coatings within a few days. Depending on the residual gas concentration in the vacuum environment, surface deposition of carbon during the exposure lead to losses in the multilayer reflectivity. However, in none of the experimental runs was structural damage within the bulk of the multilayers observed. Mo/Si multilayer coatings recovered their full original reflectivity after removal of the carbon layer by an ozone cleaning method. Auger depth profiling on Mo/Be multilayers indicate that carbon penetrated into the Be top layer during illumination with high doses of EUV radiation. Subsequent ozone cleaning fully removed the carbon, but revealed enhanced oxidation of the area illuminated, which led to an irreversible loss in reflectance on the order of 1%.
The performance of beryllium-based multilayer coatings designed to reflect light of wavelengths near 11 nm, at normal incidence, is presented. These multilayer coatings are of special interest for extreme ultraviolet lithography (EUVL). The beryllium-based multilayers investigated were Mo/Be, Ru/Be and a new material combination Mo2C/Be. The highest reflectivity achieved so far is 70% at 11.3 nm with 70 bilayers of Mo/Be. However, even though high reflectivity is very important, there are other parameters to satisfy the requirements for an EUVL production tool. Multilayer stress, thermal stability, radiation stability and long term reflectance stability are of equal or greater importance. An experimental characterization of several coatings was carried out to determine the reflectivity, stress, microstructure, and long term stability of these coatings. Theoretically calculated reflectivities are compared with experimental results for different material pairs; differences between experimental and theoretical reflectivities and bandwidths are addressed.
Beryllium (Be) has been recently receiving considerable attention as the key material for a range of potential applications in the extreme ultraviolet (EUV) and x-ray region. Most notably, it has been successfully implemented as the spacer material in beryllium-based multilayer mirrors for EUV lithography, achieving experimental reflectivities of about 70% at wavelengths around 11.4 nm. Knowledge of the absorptive and dispersive properties of this material thus becomes important for the modeling of these optics. Experimental photoabsorption results in the region 40 - 250 eV, derived from transmission measurements on free-standing beryllium foils, are presented in this work. The measured absorption in the region extending a few tens eV below the K edge (111.7 eV) appears to be significantly (up to 50%) lower than the tabulated values. Fine structure above the K edge is also demonstrated in the measurements. These data are incorporated in an updated set for the atomic scattering factors of beryllium, obtained in the range 0.1 - 30,000 eV. Finally, the Bragg reflectivity of Mo/Be multilayer optics is modeled using the new experimental results.
Multilayer mirror coatings which reflect extreme UV (EUV) radiation are a key enabling technology for EUV lithography but must meet stringent requirements in terms of film quality, stability, and thickness control across multi optical elements up to 300 nm in diameter. Deposition technology has been dramatically improved to meet those specifications for thickness control and repeatability over large curved optical substrates. Coating uniformity was improved to +/- 0.055 percent peak-to-valley (P-V) on 140- mm flats and +/- 0.1 percent P-V across 160 mm curved substrates. the run-to-run reproducibility of the reflectance peak wavelength was improved to 0.13 percent on flats to enable fabrication of wavelength-matched sets of optics. Multilayers with reflectances of 67.5 percent at 13.42 nm and 70.2 percent at 11.34 nm are typically achieved for Mo/Si and Mo/Be multilayers, respectively. Also, we have recently achieved a reflectance of 70.1 percent at 13.5 nm for a Mo/Si multilayer deposited with a modified process. The reflectance and stress of these multilayers appear to be stable relative to the requirements for application to EUV lithography. These improvements in EUV multilayer mirror technology enable us to meet the stringent specifications for coating the large optical substrates for our next- generation EUV lithography system. The primary remaining issues are improving the run-to-run wavelength repeatability on curved optics to realize the maximum optical throughput, and verifying long-term stability of the multilayers within the environment of a production EUV lithographic system.
Multilayer mirror coatings which reflect extreme UV (EUV) radiation are a key enabling technology for EUV lithography. So/Si multilayers with reflectances of 67.5 percent at 13.4 nm are now routinely achieved and reflectances of 70.2 percent at 11.4 nm were obtained with Mo/Be multilayers. High reflectance is achieved with careful control of substrate quality, layer thicknesses, multilayer materials, interface quality, and surface termination. Reflectance and film stress were found to be stable relative to the requirements for application to EUV lithography. The run-to- run reproducibility of the reflectance peak position was characterized to be better than 0.2 percent, providing the required wavelength matching among the seven multilayer- coated mirrors used in the present lithography system design. Uniformity of coating was improved to better than 0.5 percent across 150 mm diameter substrates. These improvements in EUV multilayer mirror technology will enable us to meet the stringent specifications for coating the large optical substrates for our next-generation EUV lithography system.
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