Rossana Cambie

A 10,000 groove/mm multilayer coated grating for EUV spectroscopy

Ultra-high spectral resolution in the EUV and soft x-ray energy ranges requires the use of very high line density gratings with optimal design resulting in use of a Blazed Multilayer Grating (BMG) structure. Here we demonstrate the production of near-atomically perfect Si blazed substrates with an ultra-high groove density (10,000 l/mm) together with the measured and theoretical performance of an Al/Zr multilayer coating on the grating. A 1st order absolute efficiency of 13% and 24.6% was achieved at incidence angles of 11° and 36° respectively. Cross-sectional TEM shows the effect of smoothing caused by the surface mobility of deposited atoms and we correlate this effect with a reduction in peak diffraction efficiency. This work shows the high performance that can be achieved with BMGs based on small-period anisotropic etched Si substrates, but also the constraints imposed by the surface mobility of deposited species.

High-efficiency 5000 lines/mm multilayer-coated blazed grating for extreme ultraviolet wavelengths

Volume x-ray gratings consisting of a multilayer coating deposited on a blazed substrate can diffract with very high efficiency, even in high orders if diffraction conditions in-plane (grating) and out-of-plane (Bragg multilayer) are met simultaneously. This remarkable property, however, depends critically on the ability to create a structure with near atomic perfection. In this Letter we report on a method to produce these structures. We report measurements that show, for a 5000l/mm grating diffracting in the third order, a diffraction efficiency of 37.6% at a wavelength of 13.6nm. This work now shows a direct route to achieving high diffraction efficiency in high order at wavelengths throughout the soft x-ray energy range.

Design of a hybrid double-sideband/single-sideband (schlieren) objective aperture suitable for electron microscopy.

A novel design is described for an aperture that blocks a half-plane of the electron diffraction pattern out to a desired scattering angle, and then--except for a narrow support beam--transmits all of the scattered electrons beyond that angle. Our proposed tulip-shaped design is thus a hybrid between the single-sideband (ssb) aperture, which blocks a full half-plane of the diffraction pattern, and the conventional (i.e. fully open) double-sideband (dsb) aperture. The benefits of this hybrid design include the fact that such an aperture allows one to obtain high-contrast images of weak-phase objects with the objective lens set to Scherzer defocus. We further demonstrate that such apertures can be fabricated from thin-foil materials by milling with a focused ion beam (FIB), and that such apertures are fully compatible with the requirements of imaging out to a resolution of at least 0.34nm. As is known from earlier work with single-sideband apertures, however, the edge of such an aperture can introduce unwanted, electrostatic phase shifts due to charging. The principal requirement for using such an aperture in a routine data-collection mode is thus to discover appropriate materials, protocols for fabrication and processing and conditions of use such that the hybrid aperture remains free of charging over long periods of time.

Minimizing electrostatic charging of an aperture used to produce in-focus phase contrast in the TEM

Microfabricated devices designed to provide phase contrast in the transmission electron microscope must be free of phase distortions caused by unexpected electrostatic effects. We find that such phase distortions occur even when a device is heated to 300 °C during use in order to avoid the formation of polymerized, carbonaceous contamination. Remaining factors that could cause unwanted phase distortions include patchy variations in the work function of a clean metal surface, radiation-induced formation of a localized oxide layer, and creation of a contact potential between an irradiated area and the surround due to radiation-induced structural changes. We show that coating a microfabricated device with evaporated carbon apparently eliminates the problem of patchy variation in the work function. Furthermore, we show that a carbon-coated titanium device is superior to a carbon-coated gold device, with respect to radiation-induced electrostatic effects. A carbon-coated, hybrid double-sideband/single-sideband aperture is used to record in-focus, cryo-EM images of monolayer crystals of streptavidin. Images showing no systematic phase error due to charging are achievable under conditions of low-dose data collection. The contrast in such in-focus images is sufficient that one can readily see individual streptavidin tetramer molecules. Nevertheless, these carbon-coated devices perform well for only a limited length of time, and the cause of failure is not yet understood.

High-efficiency multilayer blazed gratings for EUV and soft x-rays: recent developments

Multilayer coated blazed gratings with high groove density are the best candidates for use in high resolution EUV and soft x-ray spectroscopy. Theoretical analysis shows that such a grating can be potentially optimized for high dispersion and spectral resolution in a desired high diffraction order without significant loss of diffraction efficiency. In order to realize this potential, the grating fabrication process should provide a perfect triangular groove profile and an extremely smooth surface of the blazed facets. Here we report on recent progress achieved at the Advanced Light Source (ALS) in fabrication of high quality multilayer coated blazed gratings. The blazed gratings were fabricated using scanning beam interference lithography followed by wet anisotropic etching of silicon. A 200 nm period grating coated with a Mo/Si multilayer composed with 30 bi-layers demonstrated an absolute efficiency of 37.6% in the 3rd diffraction order at 13.6 nm wavelength. The groove profile of the grating was thoroughly characterized with atomic force microscopy before and after the multilayer deposition. The obtained metrology data were used for simulation of the grating efficiency with the vector electromagnetic PCGrate-6.1 code. The simulations showed that smoothing of the grating profile during the multilayer deposition is the main reason for efficiency losses compared to the theoretical maximum. Investigation of the grating with cross-sectional transmission electron microscopy revealed a complex evolution of the groove profile in the course of the multilayer deposition. Impact of the shadowing and smoothing processes on growth of the multilayer on the surface of the sawtooth substrate is discussed.

Development of pseudorandom binary arrays for calibration of surface profile metrology tools

Optical metrology tools, especially for short wavelengths (extreme ultraviolet and x-ray), must cover a wide range of spatial frequencies from the very low, which affects figure, to the important mid-spatial frequencies and the high spatial frequency range, which produces undesirable scattering. A major difficulty in using surface profilometers arises due to the unknown point-spread function (PSF) of the instruments [G. D. Boreman, Modulation Transfer Function in Optical and Electro-Optical Systems (SPIE, Bellingham, WA, 2001)] that is responsible for distortion of the measured surface profile. Generally, the distortion due to the PSF is difficult to account for because the PSF is a complex function that comes to the measurement via the convolution operation, while the measured profile is described with a real function. Accounting for instrumental PSF becomes significantly simpler if the result of measurement of a profile is presented in the spatial frequency domain as a power spectral density (PSD) distr...

Calibration of the modulation transfer function of surface profilometers with binary pseudorandom test standards: expanding the application range to Fizeau interferometers and electron microscopes

A modulation transfer function (MTF) calibration method based on binary pseudorandom (BPR) gratings and arrays has been proven to be an effective MTF calibration method for interferometric microscopes and a scatterometer. Here we report on a further expansion of the application range of the method. We describe the MTF calibration of a 6 in. phase shifting Fizeau interferometer. Beyond providing a direct measurement of the interferometers MTF, tests with a BPR array surface have revealed an asymmetry in the instruments data processing algorithm that fundamentally limits its bandwidth. Moreover, the tests have illustrated the effects of the instruments detrending and filtering procedures on power spectral density measurements. The details of the development of a BPR test sample suitable for calibration of scanning and transmission electron microscopes are also presented. Such a test sample is realized as a multilayer structure with the layer thicknesses of two materials corresponding to the BPR sequence. The investigations confirm the universal character of the method that makes it applicable to a large variety of metrology instrumentation with spatial wavelength bandwidths from a few nanometers to hundreds of millimeters.

Stability of modulation transfer function calibration of surface profilometers using binary pseudo-random gratings and arrays with nonideal groove shapes

Stability of modulation transfer function calibration of surface profilometers using binary pseudo-random gratings and arrays with non-ideal groove shapes Samuel K. Barber Lawrence Berkeley National Laboratory, 1 Cyclotron Road, M/S 2R0400, Berkeley, CA 94720-8199, USA +1-510-486-4077 TEL +1-510-486-7696 FAX Email address: SBarber@lbl.gov Erik H. Anderson Lawrence Berkeley National Laboratory, 1 Cyclotron Road, M/S 2R0400, Berkeley, CA 94720-8199, USA +1-510-486-4446 TEL +1-510-486-4955FAX Email address: EHAnderson@lbl.gov Rossana Cambie Lawrence Berkeley National Laboratory, 1 Cyclotron Road, 46R0125,

Fabrication and characterization of a new high density Sc/Si multilayer sliced grating

State of the art soft x-ray spectroscopy techniques like Resonant Inelastic X-ray Scattering (RIXS) require diffraction gratings which can provide extremely high spectral resolution of 105-106. This problem may be addressed with a sliced multilayer grating with an ultra-high groove density (up to 50,000 mm-1) proposed in the recent publication [Voronov, D. L., et al., Proc. SPIE 6705, 67050E (2007)]. It has been suggested to fabricate such a grating by deposition of a soft x-ray multilayer on a substrate which is a blazed saw-tooth grating (echellette) with low groove density. Subsequent polishing applied to the coated grating removes part of the coating and forms an oblique-cut multiline structure that is a sliced multilayer grating. The resulting grating has a short-scale periodicity of lines (bilayers), which is defined by the multilayer period and the oblique-cut angle. We fabricated and tested a Sc/Si multilayer sliced grating suitable for EUV applications, which is a first prototype based on the suggested technique. In order to fabricate an echellette substrate, we used anisotropic KOH etching of a Si wafer. The etching regime was optimized to obtain smooth and flat echellette facets. A Sc/Si multilayer was deposited by dc-magnetron sputtering, and after that it was mechanically polished using a number of diamond pastes. The resulting sliced grating prototype with ~270 nm line period has demonstrated a dispersive ability in the 41-49 nm photon wavelength range with a diffraction efficiency of ~7% for the optimized 38th order assigned to the echellette grating of 10 μm period.

Roughening and smoothing behavior of Al/Zr multilayers grown on flat and saw-tooth substrates

Diffraction gratings with high efficiency and high groove density are required for EUV and soft x-ray spectroscopy techniques (such as Resonant Inelastic X-ray Scattering, RIXS) designed for state-of-the-art spectral resolution and throughput. A multilayer coated blazed grating (MBG) fabricated by deposition of a multilayer on a saw-tooth substrate could address these challenges. In order to obtain high diffraction efficiency one should provide perfect triangular grooves on a substrate and perfect replication of the groove profile during the multilayer deposition. However, multilayers trend to smooth out the corrugated surface of the substrates, resulting in the main limiting factor for efficiency of ultra-dense MBGs. Understanding of the growth of multilayers on saw-tooth substrates is a key for further grating improvement. In this work we investigate growth behavior of Al/Zr multilayers on saw-tooth substrates with a groove density of 10,000 lines/mm. We apply existing growth models to describe an evolution of Power Spectral Density functions of a grating surface during the multilayer deposition, and identify a main smoothing mechanism. We found that growth of flat multilayers is well modeled with surface diffusion caused by surface curvature as a main relaxation mechanism, while growth of the multilayer on saw-tooth substrates obeys different kinetics. Limitations of the linear approach and possible model improvements by accounting for an additional component of the surface diffusion flux, caused by a gradient of adatom concentration on a corrugated surface are discussed.