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A blazed diffraction grating for the EUV lithography Beamline 12.0.1 of the Advanced Light Source has been fabricated using optical direct write lithography and anisotropic wet etching technology. A variable line spacing pattern was recorded on a photoresist layer and transferred to a hard mask layer of the grating substrate by a plasma etch. Then anisotropic wet etching was applied to shape triangular grating grooves with precise control of the ultralow blaze angle. Variation of the groove density along the grating length was measured with a Long Trace Profiler (LTP). Fourier analysis of the LTP data confirmed high groove placement accuracy of the grating. The grating coated with a Ru coating demonstrated diffraction efficiency of 69.6% in the negative first diffraction order which is close to theoretical efficiency at the wavelength of 13.5 nm. This work demonstrates an alternative approach to fabrication of highly efficient and precise x-ray diffraction gratings with ultra-low blaze angles.

A Variable Line Spacing (VLS) diffraction grating has been fabricated using an optical direct write technique. This grating is now in use at the Advanced Light Source, in beamline 12.0.1, delivering light for EUV lithography. Direct Write Lithography (DWL) with focused light at λ = 442 nm was used for the first time to record a VLS grating pattern on a substrate coated with a photoresist. The pattern was transferred to the Si substrate surface using reactive plasma etch. Precision of groove placement was verified by wavefront measurements of a witness grating recorded simultaneously with the VLS pattern. Atomic force microscope measurements confirmed near ideal groove shape and high smoothness of the grating grooves. The grating coated with a Ru coating demonstrated diffraction efficiency of 39.5% in the negative first diffraction order which corresponds to theoretical efficiency at the wavelength of 13.5 nm. This work validates the DWL approach as a promising technique for advanced grating fabrication.

MAESTRO, the Microscopic and Electronic STRucture Observatory, currently under construction at the Advanced Light Source (ALS), will be a world premier facility for the study of electronic and structural properties of in situ grown crystals. The new facility will be comprised of several end-stations, including angle-resolved photoemission spectroscopy, μARPES and nARPES end-stations, and a photoemission electron microscope combined with a lowenergy electron microscope (PEEM/LEEM). Redirection of the x-ray beam between the μARPES and PEEM/LEEM end-stations, which are longitudinally separated by 2.5 meters, uses a system of two bendable mirrors, placed in Kirkpatrick-Baez configuration designed for two foci. Here we present the details of the mirrors’ design and report on the characterization of the mirrors carried out at the ALS X-ray optical laboratory (XROL). Optimal tuning and calibration of the mirrors was performed using a technique recently developed at the OML [Opt. Eng. 48(8), 083601 (2009)]. The technique is based on regression analysis of surface slope data obtained with a long trace profiler (LTP). We provide results of tests of temporal and temperature stabilities of the shape of the mirrors. High reliability of the optical metrology with the mirrors has become possible due to a modification of the tuning procedure described in the present article. The modification allows accounting for the gravity sag effect, as well as the LTP systematic error in measurements with significantly curved x-ray optics.

Fabrication of diffraction grating for x-rays is a very challenging problem due to the exacting requirements of surface quality, groove position, and groove profile. Traditional fabrication techniques have significant limitations and do not cover all the necessary requirements. For example, classical holographic recording is limited in the type of groove patterns that can be produced. This is particularly important in the design of wide aperture high resolution spectrometers, where aberration correction using complex groove patterns is necessary. We are pioneering the use of direct-write mask-less optical lithography to make grating patterns of arbitrary complexity. In this work we report on the first results from our direct-write mask-less approach, including quality assessment of the patterns using interferometric techniques.

Realizing the experimental potential of high-brightness, next generation synchrotron and free-electron laser light sources requires the development of reflecting x-ray optics capable of wavefront preservation and high-resolution nano-focusing. At the Advanced Light Source (ALS) beamline 5.3.1, we are developing broadly applicable, high-accuracy, in situ, at-wavelength wavefront measurement techniques to surpass 100-nrad slope measurement accuracy for diffraction-limited Kirkpatrick-Baez (KB) mirrors. The at-wavelength methodology we are developing relies on a series of wavefront-sensing tests with increasing accuracy and sensitivity, including scanning-slit Hartmann tests, grating-based lateral shearing interferometry, and quantitative knife-edge testing. We describe the original experimental techniques and alignment methodology that have enabled us to optimally set a bendable KB mirror to achieve a focused, FWHM spot size of 150 nm, with 1 nm (1.24 keV) photons at 3.7 mrad numerical aperture. The predictions of wavefront measurement are confirmed by the knife-edge testing. The side-profiled elliptically bent mirror used in these one-dimensional focusing experiments was originally designed for a much different glancing angle and conjugate distances. Visible-light long-trace profilometry was used to pre-align the mirror before installation at the beamline. This work demonstrates that high-accuracy, at-wavelength wavefront-slope feedback can be used to optimize the pitch, roll, and mirror-bending forces in situ, using procedures that are deterministic and repeatable.

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.

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.

Nano-focusing and brightness preservation for ever brighter synchrotron radiation and free electron laser beamlines require surface slope tolerances of x-ray optics on the order of 100 nrad. While the accuracy of fabrication and ex situ metrology of x-ray mirrors has improved over time, beamline in situ performance of the optics is often limited by application specific factors such as x-ray beam heat loading, temperature drift, alignment, vibration, etc. In the present work, we discuss the recent results from the Advanced Light Source developing high accuracy, in situ, at-wavelength wavefront measurement techniques to surpass 100-nrad accuracy surface slope measurements with reflecting x-ray optics. The techniques will ultimately allow closed-loop feedback systems to be implemented for x-ray nano-focusing. In addition, we present a dedicated metrology beamline endstation, applicable to a wide range of in situ metrology and test experiments. The design and performance of a bendable Kirkpatrick-Baez (KB) mirror with active temperature stabilization will also be presented. The mirror is currently used to study, refine, and optimize in situ mirror alignment, bending and metrology methods essential for nano-focusing application.

The next generation of synchrotrons and free electron lasers requires x-ray optical systems with extremely high-performance, generally, of diffraction limited quality. Fabrication and use of such optics requires highly accurate metrology. In the present paper, we discuss a way to improve the performance of the Long Trace Profiler (LTP), a slope measuring instrument widely used at synchrotron facilities to characterize x-ray optics at high-spatial-wavelengths from approximately 2 mm to 1 m. One of the major sources of LTP systematic error is the detector. For optimal functionality, the detector has to possess the smallest possible pixel size/spacing, a fast method of shuttering, and minimal nonuniformity of pixel-to-pixel photoresponse. While the first two requirements are determined by choice of detector, the non-uniformity of photoresponse of typical detectors such as CCD cameras is around 2-3%. We describe a flat-field calibration setup specially developed for calibration of CCD camera photo-response and dark current with an accuracy of better than 0.5%. Such accuracy is adequate for use of a camera as a detector for an LTP with performance of ~0.1 microradian (rms). We also present the design details of the calibration system and results of calibration of a DALSA CCD camera used for upgrading our LTP-II instrument at the ALS Optical Metrology Laboratory.

Micro-focusing is widely applied at soft and hard x-ray wavelengths. One typical method, in addition to zone plates, is to split the focusing in the tangential and sagittal directions into two elliptically cylindrical reflecting elements, the so-called Kirkpatrick-Baez (KB) pair. In the simplest case each optic is made by grinding and polishing a flat, and applying unequal bending couples to each end. After briefly reviewing the nature of the bending, we show two new methods for optimal adjustment of these mirror systems using our surface normal slope measuring instrument, the long trace profiler (LTP). First, we adapt a method previously used to adjust mirrors on synchrotron radiation beamlines. We measure the slope of the surface before and after a single small adjustment of each bending couple. This permits an approximation to the functional dependence of slope on the adjustments, and allows, by applying the results of a simple matrix calculation, direct adjustment to a nearly final setting. Typically, the near linearity of the problem determines a very fast convergence of the adjustment procedure. Second, we subdivide the slope data from the LTP into three regions on the mirror, and fit a circle to each sub-region by regression. This method also allows rapid iterative adjustment of both bending couples. We show that this method is a particular case of the first one. As an overall indicator of predicted performance, we ray trace, using profiler data, predicting the exact optical performance to be expected during use of the system.

The consistency of different instruments and methods for measuring two-dimensional (2D) power spectral density (PSD) distributions are investigated. The instruments are an interferometric microscope, an atomic force microscope (AFM) and the X-ray Reflectivity and Scattering experimental facility, all available at Lawrence Berkeley National Laboratory. The measurements were performed with a gold-coated mirror with a highly polished stainless steel substrate. It was shown that these three techniques provide essentially consistent results. For the stainless steel mirror, an envelope over all measured PSD distributions can be described with an inverse power-law PSD function. It is also shown that the measurements can be corrected for the specific spatial frequency dependent systematic errors of the instruments. The AFM and the X-ray scattering measurements were used to determine the modulation transfer function of the interferometric microscope. The corresponding correction procedure is discussed in detail. Lower frequency investigation of the 2D PSD distribution was also performed with a long trace profiler and a ZYGO GPI interferometer. These measurements are in some contradiction, suggesting that the reliability of the measurements has to be confirmed with additional investigation. Based on the crosscheck of the performance of all used methods, we discuss the ways for improving the 2D PSD characterization of X-ray optics.