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The optical design of a two-dimensional imaging soft X-ray spectrometer is described. A monochromator will produce a dispersed spectrum in a narrow vertical illuminated stripe (∼2 µm wide by ∼2 mm tall) on a sample. The spectrometer will use inelastically scattered X-rays to image the extended field on the sample in the incident photon energy direction (vertical), resolving the incident photon energy. At the same time it will image and disperse the scattered photons in the orthogonal (horizontal) direction, resolving the scattered photon energy. The principal challenge is to design a system that images from the flat-field illumination of the sample to the flat field of the detector and to achieve sufficiently high spectral resolution. This spectrometer provides a completely parallel resonant inelastic X-ray scattering measurement at high spectral resolution (∼30000) over the energy bandwidth (∼5 eV) of a soft X-ray absorption resonance.

Multilayer coated blazed gratings with high groove density are the most promising candidate for ultra-high resolution soft x-ray spectroscopy. They combine the ability of blazed gratings to concentrate almost all diffraction energy in a desired high diffraction order with high reflectance soft x-ray multilayers. However in order to realize this potential, the grating fabrication process should provide a near perfect groove profile with an extremely smooth surface of the blazed facets. Here we report on successful fabrication and testing of ultra-dense saw-tooth substrates with 5,000 and 10,000 lines/mm.

At the Advanced Light Source (ALS), we are developing broadly applicable, high-accuracy, in-situ, at-wavelength wavefront slope measurement techniques for Kirkpatrick-Baez (KB) mirror nano-focusing. In this paper, we report an initial cross-check of ex-situ and in-situ metrology of a bendable temperature stabilized KB mirror. This cross-check provides a validation of the in-situ shearing interferometry currently under development at the ALS.

Super high quality aspherical x-ray mirrors with a residual slope error of ∼100 nrad (root-mean-square) and a height error of ∼1-2 nm (peak-to-valley), and even lower, are now available from a number of the most advanced vendors utilizing deterministic polishing techniques. The mirror specification for the fabrication is based on the simulations of the desired performance of the mirror in the beamline optical system and is normally given with the acceptable level of deviation of the mirror figure and finish from the desired ideal shape. For example, in the case of aspherical x-ray mirrors designed for the Advanced Light Source (ALS) QERLIN beamline, the ideal shape is defined with the beamline application (conjugate) parameters and their tolerances. In this paper, we first discuss an original procedure and dedicated software developed at the ALS X-Ray Optics Laboratory (XROL) for optimization of beamline performance of pre-shaped hyperbolic and elliptical mirrors. The optimization is based on results of ex situ surface slope metrology and consists in minimization of the mirror shape error by determining the conjugate parameters of the best-fit ideal shape within the specified tolerances. We describe novel optical metrology instrumentation, measuring techniques, and analytical methods used at the XROL for acquisition of surface slope data and optimization of the optic's beamline performance. The high efficacy of the developed experimental methods and data analysis procedures is demonstrated in results of measurements with and performance optimization of hyperbolic and elliptical cylinder mirrors designed and fabricated for the ALS QERLIN beamline.

We present details of design of elliptically bent Kirkpatrick-Baez mirrors developed and successfully used at the advanced light source for submicron focusing. A distinctive feature of the mirror design is an active temperature stabilization based on a Peltier element attached directly to the mirror body. The design and materials have been carefully optimized to provide high heat conductance between the mirror body and substrate. We describe the experimental procedures used when assembling and precisely shaping the mirrors, with special attention paid to laboratory testing of the mirror-temperature stabilization. For this purpose, the temperature dependence of the surface slope profile of a specially fabricated test mirror placed inside a temperature-controlled container was measured. We demonstrate that with active mirror-temperature stabilization, a change of the surrounding temperature by more than 3 K does not noticeably affect the mirror figure. Without temperature stabilization, the rms slope error is changed by approximately 1.5 μrad (primarily defocus) under the same conditions.

The purpose of this document is to outline the Advanced Light Source (ALS) approach for preventing a radiation accident scenario on the ALS experimental floor due to top-off operation. The document will describe the potential risks, the analysis, and the resulting specifications for the controls.

Two new soft X-ray scanning transmission microscopes located at the Advanced Light Source (ALS) have been designed, built and commissioned. Interferometer control implemented in both microscopes allows the precise measurement of the transverse position of the zone plate relative to the sample. Long-term positional stability and compensation for transverse displacement during translations of the zone plate have been achieved. The interferometer also provides low-distortion orthogonal x, y imaging. Two different control systems have been developed: a digital control system using standard VXI components at beamline 7.0, and a custom feedback system based on PC AT boards at beamline 5.3.2. Both microscopes are diffraction limited with the resolution set by the quality of the zone plates. Periodic features with 30 nm half period can be resolved with a zone plate that has a 40 nm outermost zone width. One microscope is operating at an undulator beamline (7.0), while the other is operating at a novel dedicated bending-magnet beamline (5.3.2), which is designed specifically to illuminate the microscope. The undulator beamline provides count rates of the order of tens of MHz at high-energy resolution with photon energies of up to about 1000 eV. Although the brightness of a bending-magnet source is about four orders of magnitude smaller than that of an undulator source, photon statistics limited operation with intensities in excess of 3 MHz has been achieved at high energy resolution and high spatial resolution. The design and performance of these microscopes are described.

The high brightness of the bend magnets at the Advanced Light Source has been exploited to illuminate a scanning transmission X-ray microscope (STXM). This is the first diffraction-limited scanning X-ray microscope to operate with a useful count rate on a synchrotron bend-magnet source. A simple dedicated beamline has been built covering the range of photon energy from 250 eV to 600 eV. The beamline is always available and needs little adjustment. Use of this facility is much easier than that of installations that share undulator beams. This facility provides radiation for C 1s, N 1s and O 1s near-edge X-ray absorption spectromicroscopy with STXM count rates in excess of 1 MHz and with spectral resolution typically 1:2000, limited to about 1:5000.

At the Advanced Light Source (ALS), we are developing broadly applicable, high-accuracy, in situ, at-wavelength wavefront slope measurement techniques for Kirkpatrick-Baez (KB) mirror nano-focusing. We describe here details of the metrology beamline endstation, the at-wavelength tests, and an original alignment method that have already allowed us to precisely set a bendable KB mirror to achieve a FWHM focused spot size of ~;;120 nm, at 1-nm soft x-ray wavelength.

A new beam line (beam line 11.0) at the Advanced Light Source has been designed to employ an SX700 (Peterson, Opt. Commun. 40 (1982) 402) style variable-included-angle plane-grating-monochromator. The extended range available from a specific grating is exploited to cover energies from the carbon 1 s absorption edge to the oxygen 1 s absorption edge with two different gratings (150 and 1200 lines/mm) with dispersion different by a factor of three. The phase space of a zone plate microscope can then be efficiently filled either at low or high resolution (R=2500 and 7500). At the same time the monochromator is designed to cover the energy range from 75 to 1500 eV using the same two gratings at high resolution for spectroscopy. A deformable mirror pair will re-focus to a monochromatic spot 5×10 μm, matched into the acceptance of a fluorescence spectrometer. The monochromator will operate in vertically collimated light and the free choice of focussing parameter provides a guarantee of high resolution even when the power loading is high. However, we will provide a thermally engineered pre-mirror so that the high resolution requirement at low photon energy can be met without loss of efficiency.

The design of VUV beamlines for the Advanced Light Source is discussed. Features of the design serve to illustrate the careful attention required in order to preserve the performance of the low emittance “third-generation” storage ring, operating with insertion devices.

The U8 is a beam line under construction at the Advanced Light Source (ALS). The beam line will be described along with calculations of its performance and its current status. An 8 cm period undulator is followed by two spherical collecting mirrors, an entrance slit, spherical gratings having a 15{degree} deviation angle, a moveable exit slit, and refocusing and branching mirrors. Internal water cooling is provided to the metal M1 and M2 mirrors as well as to the gratings. Calculations have been made of both the flux output and the resolution over its photon energy range of 20--300 eV. The design goal was to achieve high intensity, 10{sup 12} photons/sec, at a high resolving power of 10,000. The U8 Participating Research Team (PRT) is planning experiments involving the photoelectron spectroscopy of gaseous atoms and molecules, the spectroscopy of ions and actinide spectroscopy.

Design criteria are described, and test results are presented, for prototype undulator beam position monitors at the Advanced Light Source (ALS). The design is based on monitors presently in use at the National Synchrotron Light Source, Brookhaven National Laboratory, with modifications to account for the widely varying and large K values of the undulators to be installed at the ALS. In particular, we have modified the design to simplify the thermal engineering and we have explored techniques to suppress the response of the monitors to soft photons, below 100 eV, so that the beam position can be determined by measuring the higher energy photons which are better collimated.

We have studied the effects of temperature fluctuations on the Advanced Light Source (ALS). By modeling the storage ring support structure, we find that fluctuations of ± 2 to 3°C in the tunnel will cause photon beam motion of the order of the beam size. Temperature stabilization at this level will allow the residual motion of the photon beams to be reduced by a second level of active feedback, operating on signals from photon beam position monitors. Air temperature in the experimental area and the temperature of cooling water serving the beamlines should be constant to ± 1°C. This will provide a suitable environment for experiments.

The development of two zone-plate microscopes for X-ray spectroscopic analysis of materials is described. This pair of instruments will provide imaging NEXAFS analysis of samples in transmission at atmospheric pressure and imaging XPS and NEXAFS analysis of sample surfaces in a UHV environment.

Position monitors are implemented in three undulator beamlines at the ALS. Their performance has been studied carefully on one of these lines and is reviewed. The monitors work as expected and show the ALS to be an exceptionally stable source of synchrotron radiation.

The interaction of single cell microorganisms with inorganic substrates is a central issue in soil and aquatic environmental chemistry. The biochemical pathways of the bacterial metabolism based on redox reactions of transition metal compounds involve the processes of microbial attachment to and subsequent modification of inorganic surfaces (biocorrosion), as well as the precipitation of inorganic compounds (biomineralization). Soft x-ray spectromicroscopy has been used to investigate Mn micronodules collected from freshwater sediments in order to attempt the direct mapping of the distribution of Mn valence states in biologically produced minerals.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

The SpectroMicroscopy Facility at the Advanced Light Source is based on a high brightness, high‐resolution beamline, and includes a collection of projects designed to exploit the unique characteristics of the soft x‐ray beam. The beamline itself is comprised of a 5‐m long, 5‐cm‐period undulator, a spherical‐grating monochromator with water‐cooled gratings. Adaptive optics refocus the monochromatic beam to two ‘‘microfocus’’ experimental stations with spot sizes less than 50 μm diameter and a third ‘‘nanofocus’’ station uses a zone‐plate lens to further demagnify the microfocus spot. Experimental stations include an ‘‘ultraESCA’’ spectrometer for small‐area spectroscopy and photoelectron diffraction, a scanning transmission x‐ray microscope, and photoelectron microscopes. Commissioning experiments of microscopic actinide photoemission, surface‐core‐level photoelectron diffraction, and high‐resolution soft x‐ray fluorescence demonstrate dramatic improvements in sensitivity due to the high brightness and sma...

A new facility for microdiffraction strain measurements and microfluorescence mapping has been built on beamline 12.3.2 at the advanced light source of the Lawrence Berkeley National Laboratory. This beamline benefits from the hard x-radiation generated by a 6 T superconducting bending magnet (superbend). This provides a hard x-ray spectrum from 5 to 22 keV and a flux within a 1 microm spot of approximately 5x10(9) photons/s (0.1% bandwidth at 8 keV). The radiation is relayed from the superbend source to a focus in the experimental hutch by a toroidal mirror. The focus spot is tailored by two pairs of adjustable slits, which serve as secondary source point. Inside the lead hutch, a pair of Kirkpatrick-Baez (KB) mirrors placed in a vacuum tank refocuses the secondary slit source onto the sample position. A new KB-bending mechanism with active temperature stabilization allows for more reproducible and stable mirror bending and thus mirror focusing. Focus spots around 1 microm are routinely achieved and allow a variety of experiments, which have in common the need of spatial resolution. The effective spatial resolution (approximately 0.2 microm) is limited by a convolution of beam size, scan-stage resolution, and stage stability. A four-bounce monochromator consisting of two channel-cut Si(111) crystals placed between the secondary source and KB-mirrors allows for easy changes between white-beam and monochromatic experiments while maintaining a fixed beam position. High resolution stage scans are performed while recording a fluorescence emission signal or an x-ray diffraction signal coming from either a monochromatic or a white focused beam. The former allows for elemental mapping, whereas the latter is used to produce two-dimensional maps of crystal-phases, -orientation, -texture, and -strain/stress. Typically achieved strain resolution is in the order of 5x10(-5) strain units. Accurate sample positioning in the x-ray focus spot is achieved with a commercial laser-triangulation unit. A Si-drift detector serves as a high-energy-resolution (approximately 150 eV full width at half maximum) fluorescence detector. Fluorescence scans can be collected in continuous scan mode with up to 300 pixels/s scan speed. A charge coupled device area detector is utilized as diffraction detector. Diffraction can be performed in reflecting or transmitting geometry. Diffraction data are processed using XMAS, an in-house written software package for Laue and monochromatic microdiffraction analysis.

Phase segregation is important in determining the physical and chemical properties of many complex polymers, including polyurethanes. Achieving a better understanding of the connections between formulation chemistry, the chemical nature of segregated phases, and the physical properties of the resulting polymer, has the potential to greatly advance the development of improved polyurethane materials. However, the sub-micron size of segregated features precludes their chemical analysis by most existing methods. Near edge X-ray absorption spectroscopy carried out with sub micron spatial resolution provides one of the few suitable means for quantitative chemical analysis (speciation) of individual segregated phases. We have used the NSLS and ALS scanning transmission x-ray microscopes (STXM) to record images and spectra of both model and real polyurethane polymers. Relative to energy loss spectroscopy in a transmission electron microscope, STXM has remarkable advantages with regard to a much lower radiation damage rates and much higher spectral resolution (∼0.1 eV at the C ls edge), with a spatial resolution (∼0.1 μm) adequate for many real world problems in polymer analysis.

Two new scanning x-ray transmission microscopes are being built at beamline 5.3.2 and beamline 7.0 of the Advanced Light Source that have novel aspects in their control and acquisition systems. Both microscopes use multiaxis laser interferometry to improve the precision of pixel location during imaging and energy scans as well as to remove image distortions. Beam line 5.3.2 is a new beam line where the new microscope will be dedicated to studies of polymers in the 250–600 eV energy range. Since this is a bending magnet beam line with lower x-ray brightness than undulator beam lines, special attention is given to the design not only to minimize distortions and vibrations but also to optimize the controls and acquisition to improve data collection efficiency. 5.3.2 microscope control and acquisition is based on a PC computer running WINDOWS 2000. All mechanical stages are moved by stepper motors with rack mounted controllers. A dedicated counter board is used for counting and timing and a multi-input/output...

Some tests have been made of phosphors for photon beam diagnosis. Plasma‐sprayed coatings were checked for damage and decay during a period of several ampere hours of irradiation from the x‐ray ring at the National Synchrotron Light Source. Surface temperatures were measured and extrapolated to give an indication of the temperatures expected in more powerful photon beams. Based on our findings we have chosen plasma‐sprayed coatings of europium‐doped yttrium oxide as the best candidate for use on masks and flags in ‘‘white’’ photon beams of the new facilities.