Ion-beam figuring (IBF) capable of providing sub-nanometer shape accuracy, is often used for fabrication of ultra-precise x-ray optics. However, in the case of gratings, the optical surface may degrade during the following ruling procedure or etching processes. This leads to the necessity for a post-ruling surface correction to recover the ultra-precise shape of the optics, while the IBF substrate finish prior the ruling could be omitted. If so, the gratings can be made using relatively inexpensive substrates produced with conventional mechanical or chemical-mechanical polishing with medium optical surface quality and then processed with a post-ruling IBF to bring the shape to the sub-nanometer accuracy. The key question is whether the grating grooves survive the IBF treatment. In this work we investigate the possibility of post-production IBF correction for lamellar x-ray gratings. A 200 lines/mm lamellar grating made using a lambda/20 Si substrate was processed with IBF to achieve a sub-nanometer flat optical surface of the final grating. We report on impact of the IBF process on groove profile, surface roughness, and diffraction efficiency of the grating.
We developed a new process for low blaze angle (LBA) diffraction gratings for x-ray applications. The process provides a perfect shape of the saw-tooth grooves and preserves high precision of the optical surface of the grating substrate. An LBA grating is made by double-replication of a master blazed grating by nanoimprinting followed by a transfer of the polymer replica into a Si grating substrate by a plasma etch. The plasma etch process optimized for a certain etch rate ratio for the polymer and Si provides a reduction of the groove depth and the blaze angle down to 0.2 degrees. The reduction results in an improvement of surface roughness compared to the master grating and mitigate process non-uniformity owing to the scaling down effect. We investigate the quality and performance of the fabricated LBA gratings and evaluate process accuracy and reproducibility. This work was supported by the US Department of Energy under contract number DE-AC02-05CH11231.
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 2 nd 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.
Low groove density gratings with blaze angles as low as 0.1‡ are required for plane grating monochromators for x-ray synchrotron and Free Electron Laser applications. To achieve so small a blaze angles we developed a process of reduction of the blaze angle of a coarse Si grating fabricated by anisotropic wet etching. The coarse grating with a blaze angle of 4° is planarized by a polymer layer and then plasma etching is applied to remove the polymer and underlying silicon material. The appropriate ratio of etch rates of Si and the polymer material provides reduction of the groove depth and the blaze angle. We developed a set of reduction recipes which provide blaze angle reduction down to 0.04° with high accuracy and which preserves the perfect triangular shape of the grooves. The ultra-low blaze angle grating coated with a Mo/Si multilayer exhibits a record diffraction efficiency of 58% due to the perfect match of the groove depth with the multilayer d-spacing. This opens up wide possibilities for making highly accurate and efficient diffraction gratings for tender x-ray, free electron laser, and EUV lithography applications. The low blaze angle gratings have a perfect triangular groove profile and highly smooth surfaces of the blazed facets which ensures high diffraction efficiency of the x-ray gratings.
The upgrade of the Advanced Light Source at Lawrence Berkeley National Lab to a Diffraction-Limited Storage Ring (DLSR) will feature four new and upgraded beamlines, designed to take full advantage of the coherence and high brightness of the insertion device source operating mostly in the soft x-ray regime (100–2000 eV). The round and highly coherent beam drives specific design choices for the photon transport optics and monochromator, and technical challenges in terms of performances, optical tolerances and stability. We have used the simulation tools Shadow (for raytracing) or SRW (wavefront propagation), and their implementation in OASYS and Sirepo to refine tolerance specifications, using their scripting capabilities and new add-ons to perform a comprehensive beamline analysis and confirm that specifications matched our performance requirements, taking into account partial coherence and issues related to heatload.
Planarization is important in many areas of nanostructure fabrication. Here we describe a new process for planarization saw-tooth surface of blazed gratings used for the monochromatization of light, but the applications should be much wider. Such gratings consist of relatively wide and very shallow triangular grooves with slanted facets which are machined with nanometer accuracy. The process of making such gratings includes planarization of a relatively coarse saw-tooth surface with micron deep grooves following by a plasma etch which provides reduction of the facet angle and hence groove depth by a factor of 10 - 100. To achieve high quality of the final grating the planarization step should provide a flat surface over the grating facets with sub-nanometer level planarity. We investigated planarization of coarse saw-tooth surfaces with a groove width of 10 μm and a facet angle of 4° by a polymer coating spun on the grating. The optimized planarization procedure provides 100% planarization even on these highly structured surfaces.
In this paper we provide an update on the development of a novel cantilevered-liquid-nitrogen-cooled-silicon mirror for a new insertion device beamline included in the Advanced Light Source Upgrade (ALS-U). The goals of this mirror development are to achieve diffraction limited performance, demonstrate reliability, minimize coolant flow induced vibration, and demonstrate carbon contamination prevention and cleaning techniques. In this paper we summarize the design requirements, the design of the mirror system, and prototype fabrication.
High diffraction efficiency of a grating can be achieved by use of inclined facets. This type of grating, normally referred to as a blazed grating, has facets that are arranged so that there is an equal angle on the incident and diffracted sides, and thus can be thought of as reflecting light into a particular order. Conventionally blazed gratings are made by diamond mechanical ruling, or more recently by anisotropic etching of silicon. However it is difficult with these processes to achieve a very low blaze angle as well as to precisely control it. This has become particularly important for applications involving Free Electron Lasers, where a very grazing incidence angle has to be used to avoid damage, and for extension of the working range up to high energies on synchrotrons. In each case, the very small angular size of the source results in a low line density, which in turn results in a low blaze angle. In high groove density multilayer blazed gratings, high precision for the blaze angle is required to match the groove depth to the multilayer d-spacing. We have developed a process which gives the possibility for alteration of the groove profile of a fabricated grating and tune the blaze angle with high precision. The method is based on planarization of the grating grooves by deposition of a SiO2 sacrificial layer followed by smoothing the surface with Ar plasma etch. Finally, a reactive plasma etching is used to etch off the sacrificial layer together with the surface layer of the Si grating. The optimized plasma etching provides a certain ratio of etch rates of the sacrificial layer and Si and results in reduction of the blaze angle down to a desired value.
We developed a process for fabrication of ultra-precise blazed diffraction gratings for high resolution x-ray spectroscopy. The process based on nanofabrication techniques provides high fidelity for groove placement, high groove density, and perfect saw-tooth profile of grating grooves. A grating pattern is recorded on a quartz plate by use of e-beam lithography with a nanometer scale accuracy over the grating size. The pattern is transferred to a grating substrate by large area nanoimprint and then a hard Cr mask is formed via a lift-off process. Fidelity of the transfer step in terms of groove placement accuracy was investigated by differential wavefront interferometry. Anisotropic wet etch was applied to the patterned Si single crystal substrate to shape triangular grooves. Fabrication of a blazed grating of area 120 mm × 30 mm with groove density of 2000 lines/mm was demonstrated.
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.
The advent of fully coherent free-electron laser and diffraction-limited synchrotron radiation storage ring sources of x-rays is catalyzing the development of new ultrahigh accuracy metrology methods. To fully exploit these sources, metrology needs to be capable of determining the figure of an optical element with subnanometer height accuracy. The major limiting factors of the current absolute accuracy of ex situ metrology are drift errors due to temporal instabilities of the lab’s environmental conditions and systematic errors inherent to the metrology instruments. Here, we discuss in detail work at the Advanced Light Source X-Ray Optics Laboratory on building of advanced environmental control that is a key component in the development of ultrahigh accuracy ex situ metrology for x-ray optics. By a few examples, we show how the improvement of the environmental conditions in the lab allows us to significantly gain efficiency in performing ex situ metrology with high-quality x-ray mirrors. The developed concepts and approaches, included in the design of the new X-Ray Optics Laboratory, are described in detail. These data are essential for construction and successful operation of a modern metrology facility for x-ray optics, as well as high-precision measurements in many fields of experimental physics.
Fernando Sannibale, Daniele Filippetto, Houjun Qian, Christos Papadopoulos, Russell Wells, Toby Kramasz, Howard Padmore, Jun Feng, James Nasiatka, Ruixuan Huang, Max Zolotorev, John Staples
After the formidable results of X-ray 4th generation light sources based on free electron lasers around the world, a new revolutionary step is undergoing to extend the FEL performance from the present few hundred Hz to MHz-class repetition rates. In such facilities, temporally equi-spaced pulses will allow for a wide range of previously non-accessible experiments. The Advanced Photo-injector EXperiment (APEX) at the Lawrence Berkeley National Laboratory (LBNL), is devoted to test the capability of a novel scheme electron source, the VHF-Gun, to generate the required electron beam brightness at MHz repetition rates. In linac-based FELs, the ultimate performance in terms of brightness is defined at the injector, and in particular, cathodes play a major role in the game. Part of the APEX program consists in testing high quantum efficiency photocathodes capable to operate at the conditions required by such challenging machines. Results and status of these tests at LBNL are presented.
The X-Ray Optics Laboratory (XROL) at the Advanced Light Source (ALS), a unique optical metrology lab, has been
recently moved to a new, dedicated clean-room facility that provides improved environmental and instrumental
conditions vitally required for high accuracy metrology with state-of-the-art X-ray optics. Besides the ALS, the XROL
serves several DOE labs that lack dedicated on-site optical metrology capabilities, including the Linac Coherent Light
Source (LCLS) at SLAC and LBNL’s Center for X-Ray Optics (CXRO). The major role of XROL is to proactively
support the development and optimal beamline use of x-ray optics. The application of different instruments available in
the lab enables separate, often complementary, investigations and addresses of different potential sources of error
affecting beamline performance. At the beamline, all the perturbations combine to produce a cumulative effect on the
performance of the optic that makes it difficult to optimize the optic's operational performance. Ex situ metrology allows
us to address the majority of the problems before the installation of the optic at a beamline, and to provide feedback on
design and guidelines for the best usage of optics. We will review the ALS XROL mission, lab design and arrangement,
ex situ metrology capabilities and performance, as well as the future plans for instrumentation upgrades. The discussion
will be illustrated with the results of a broad spectrum of measurements of x-ray optics and optical systems performed at
the XROL.
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.
Junqi Xie, Marcel Demarteau, Robert Wagner, Miguel Ruiz-Oses, Xue Liang, Ilan Ben-Zvi, Klaus Attenkofer, Susanne Schubert, John Smedley, Jared Wong, Howard Padmore, Arthur Woll
Bi-alkali antimonide photocathode is an essential component in fast timing response photomultipliers. Real-time in-situ grazing incidence x-ray diffraction and post-growth x-ray reflectivity measurement were performed to study the photocathode deposition process on glass substrate. Grazing incidence x-ray diffraction patterns show the formation of Sb crystalline, dissolution of crystalline phase Sb by the application of K vapor and reformation of refined crystal textures. XRR result exhibits that the film thickness increases ~ 4.5 times after K diffusion and almost have no change after Cs diffusion. Further investigation is expected to understand the photocathode growth process and provide guidelines for photocathode development.
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.
Junqi Xie, Marcel Demarteau, Robert Wagner, Edward May, Jiang Zhang, Miguel Ruiz-Oses, Xue Liang, Ilan Ben-Zvi, Klaus Attenkofer, Susan Schubert, John Smedley, Jared Wong, Howard Padmore
The development of X-ray techniques opens new opportunities for real-time in-situ study of photocathode growth
process in details. The initial ultra thin Sb films during photocathode process were investigated on multiple substrates
based on different applications. The real-time X-ray scattering and post-growth X-ray reflectivity and diffraction
measurement were performed and analyzed. Experiment results indicate that Sb deposition performs a phase change
from amorphous to crystalline, the critical thicknesses are different on B33 float glass, Si and Mo. Two methods were
applied for film thickness calculation from X-ray scattering data, and they agree well with thickness monitor result. Sb
films deposited on different substrates show similar final film roughnesses. The real time x-ray study indicates that the
initial Sb layer deposition process on different substrate has different structure during deposition, the optimized
thickness of the initial Sb layer may varies depends on the substrate. This study also paved the road for further study of
the more complex alkali metal vapor diffusion process in photocathode growth.
We demonstrate a comprehensive and broadly applicable methodology for the optimal in situ configuration of bendable soft x-ray Kirkpatrick-Baez mirrors. The mirrors used for this application are preset at the Advanced Light Source Optical Metrology Laboratory prior to beamline installation. The in situ methodology consists of a new technique for simultaneously setting the height and pitch angle of each mirror. The benders of both mirrors were then optimally tuned in order to minimize ray aberrations to a level below the diffraction-limited beam waist size of 200 nm (horizontal)×100 nm (vertical) . After applying this methodology, we measured a beam waist size of 290 nm (horizontal)×130 nm (vertical) with 1 nm light using the Foucault knife-edge test. We also discuss the utility of using a grating-based lateral shearing interferometer with quantitative wavefront feedback for further improvement of bendable optics.
We demonstrate a comprehensive and broadly applicable methodology for the optimal in situ configuration of bendable
soft x-ray Kirkpatrick-Baez mirrors. The mirrors used for this application are preset at the ALS Optical Metrology
Laboratory prior to beamline installation. The in situ methodology consists of a new technique for simultaneously setting
the height and pitch angle of each mirror. The benders of both mirrors were then optimally tuned in order to minimize
ray aberrations to a level below the diffraction-limited beam waist size of 200 nm (horizontal) × 100 nm (vertical). After
applying this methodology, we measured a beam waist size of 290 nm (horizontal) × 130 nm (vertical) with 1 nm light
using the Foucault knife-edge test. We also discuss the utility of using a grating-based lateral shearing interferometer
with quantitative wavefront feedback for further improvement of bendable optics.
A subwavelength plasmonic grating with rectangular grooves on the metal surface is an efficient light trapper with
designer resonance position and angular bandwidth. In this work, a new method is presented, where the grooves are
filled with a dielectric resulting in a large shift of the resonance wavelength. A case study of a gold grating with grooves
18 nm wide and 47 nm deep is presented, where the resonance is shifted from original 720 nm to 960 nm by filling the
grooves with an n = 1.4 immersion oil.
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.
We demonstrate 16 times increase in light absorption nano-structured metal compared to the flat surface by fabricating a
subwavelength grating on gold surface. This light-trapping phenomenon can be used in many areas from solar energy
conversion to photovoltaics. Here, we describe application to field enhancement in photocathodes where we show theoretically a performance increase of three orders of magnitude over conventional systems. We also describe the fabrication of these devices and present initial optical results.
When x-rays penetrate soft matter, their phase changes more rapidly than their amplitude. Interference effects
visible with high brightness sources creates higher contrast, edge enhanced images. When the object is piecewise
smooth (made of big blocks of a few components), such higher contrast datasets have a sparse solution. We
apply basis pursuit solvers to improve SNR, remove ring artifacts, reduce the number of views and radiation dose
from phase contrast datasets collected at the Hard X-Ray Micro Tomography Beamline at the Advanced Light
Source. We report a GPU code for the most computationally intensive task, the gridding and inverse gridding
algorithm (non uniform sampled Fourier transform).
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.
We report on recent progress in developing diffraction gratings which can potentially provide extremely high spectral
resolution of 105-106 in the EUV and soft x-ray photon energy ranges. Such a grating was fabricated by deposition of a
multilayer on a substrate which consists of a 6-degree blazed grating with a high groove density. The fabrication of the
substrate gratings was based on scanning interference lithography and anisotropic wet etch of silicon single crystals. The
optimized fabrication process provided precise control of the grating periodicity, and the grating groove profile, together
with very short anti-blazed facets, and near atomically smooth surface blazed facets. The blazed grating coated with 20
Mo/Si bilayers demonstrated a diffraction efficiency in the third order as high as 33% at an incidence angle of 11° and
wavelength of 14.18 nm. This work was supported by the US Department of Energy under contract number DE-AC02-05CH11231.
Modern polishing methods of ion-beam milling, and single atom removal techniques are beginning to allow the
fabrication of arbitrary surface shapes for reflecting grazing incidence optics. Moreover, the total expense of fabrication,
coating, measuring, mounting, aligning, cooling, and surrounding the optic with vacuum make the reduction of optical
part count attractive for the latest generation x-ray sources, not even considering potential effects on the scattering and
reflective losses of the radiation. These two developments converge to effectively suggest the question of what surface
would be the optimally de-magnifying surface to replace a toroid illuminated by a wave cylindrical in the sagittal
direction if the sag of the single surface were determined by a function, and not constrained to be a typical optical shape.
To address this we derive a simplified case of the formalism of Chrisp, using the classical optical path function approach
of Fermat to give a power series calculation of this best surface. This surface, the "diaboloid," would in principle earn its
name by its, at least ab initio, consideration of being very difficult to manufacture. We show an example of
improvement this surface would provide.
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.
Resonant Inelastic X-ray Scattering (RIXS) is the one of the most powerful methods for investigation of the electronic
structure of materials, specifically of excitations in correlated electron systems. However the potential of the RIXS
technique has not been fully exploited because conventional grating spectrometers have not been capable of achieving
the extreme resolving powers that RIXS can utilize. State of the art spectrometers in the soft x-ray energy range achieve
~0.25 eV resolution, compared to the energy scales of soft excitations and superconducting gap openings down to a
few meV. Development of diffraction gratings with super high resolving power is necessary to solve this problem. In
this paper we study the possibilities of fabrication of gratings of resolving power of up to 106 for the 0.5 - 1.5 KeV
energy range. This energy range corresponds to all or most of the useful dipole transitions for elements of interest in
most correlated electronic systems, i.e. oxygen K-edge of relevance to all oxides, the transition metal L2,3 edges, and the
M4,5 edges of the rare earths. Various approaches based on different kinds of diffraction gratings such as deep-etched
multilayer gratings, and multilayer coated echelettes are discussed. We also present simulations of diffraction efficiency
for such gratings, and investigate the necessary fabrication tolerances.
J. Feng, W. Wan, J. Qiang, A. Bartelt, A. Comin, A. Scholl, J. Byrd, R. Falcone, G. Huang, A. MacPhee, J. Nasiatka, K. Opachich, D. Weinstein, T. Young, H. Padmore
An ultrafast x-ray streak camera is under development at LBNL for application primarily to studies of ultrafast magnetization dynamics. In initial work, a temporal resolution of 900fs in accumulative mode at 5 KHz has been achieved. These results and methods currently being developed to improve the resolution and repetition rate are resented. One of the primary limits to temporal resolution is caused by the finite energy width of the electron distribution from the photocathode. The positive time of flight dispersion with energy in the accelerating region of the camera can be countered by introduction of downstream optics that give negative time of flight dispersion with energy, leading to an approximate overall cancellation of this temporal aberration. Initial results of an end-to-end simulation model using the full photoelectron distribution are presented.
The spin dynamics of ferromagnetic thin films following an excitation by ultrashort 100-fs near-infrared laser pulses has recently received much attention. Here, a new approach is described using x-ray magnetic circular dichroism to investigate demagnetization and magnetization switching processes. In contrast to magneto-optical measurements, x-ray dichroism has the advantage of determining separately the spin and orbital components of the magnetic moment. The relatively low time resolution of the synchrotron x-ray probe pulses (80 ps FWHM) is overcome by employing an ultrafast x-ray streak camera with a time resolution of < 1 ps. A description of the experimental setup including the x-ray/IR laser pulse synchronization and the streak camera is given.
The performance of CsI photocathodes has been characterized for use with grazing incidence soft x-rays. The total electron yield and pulsed quantum efficiency from a CsI photocathode has been measured in a reflection geometry as a function of photon energy (100 eV to 1 keV), angle of incidence and the electric field between the anode and photocathode. The total electron yield and pulsed quantum efficiency increase as the x-ray penetration depth approaches the secondary electron escape depth. Unit quantum efficiency in a grazing incidence geometry is demonstrated. A weak electric field dependence is observed for the total yield measurements; whilst no significant dependence is found for the pulsed quantum efficiency. Theoretical predictions agree accurately with experiment.
The Linac-based Ultrafast X-ray source (LUX) is a proposed recirculating linear accelerator for the purpose of producing intense, tunable, high repetition rate ultrafast x-ray pulses. An angle-time or position-time correlation is induced in the electron bunches by a dipole-mode RF cavity. Undulators and wigglers are sources of synchrotron radiation. Asymmetrically-cut crystals are used as optical elements of an x-ray pulse compression scheme. X-ray pulse durations of 50-100 fs are obtained over a range of photon energies from 2 to 12 keV. An undulator beamline consists of a collimating mirror, two asymmetric crystals and Kirkpatrick-Baez mirrors and provides compressed, monochromatic and focused x-rays for time-resolved experiments.
Although the realisation of femtosecond X-ray free electron laser (FEL) X-ray pulses is still some time away, X-ray diffraction experiments within the sub-picosecond domain are already being performed using both synchrotron and laser- plasma based X-ray sources. Within this paper we summarise the current status of some of these experiments which, to date, have mainly concentrated on observing non-thermal melt and coherent phonons in laser-irradiated semiconductors. Furthermore, with the advent of FEL sources, X-ray pulse lengths may soon be sufficiently short that the finite response time of monochromators may themselves place fundamental limits on achievable temporal resolution. A brief review of time-dependent X-ray diffraction relevant to such effects is presented.
The toroidal, silicon mirror on microdiffraction beamline 7.3.3 at the Advanced Light Source provides a 1:1 focus of the bend magnet source. The mirror is bent by two lead springs that are bolted to it through a pari of adhesive bonded end blocks. Because of the high loads that these adhesive joints must carry, three specific features of the bonds were tested: bondline geometry of the mating end blocks, surface preparation of the adherends, and strength of the adhesive. Bond strengths were evaluated by loading small test mirrors to failure using two epoxies under two different conditions of surface preparation - acid etching and simple UHV cleaning. In addition, the mirror's temperature distribution and figure errors were calculated with an Ansys Finite Element Model. The model's predictions were correlated to long trace profilometry as well as x-ray focus measurements.
A bend magnet at the advanced light source is sufficiently bright to illuminate a scanning transmission x-ray microscope, with a zone plate lens to focus the soft x-ray beam at the diffraction limit. The beam line must be carefully optimized for this one purpose of high count-rates, of the order of 1MHz, are to be achieved in the microscope. Such a design is described. The nominal resolving power is 2000 from 150eV to 600eV using a single spherical diffraction grating. Twice the resolving power is available at reduced flux, and the intensity can be traded independently against the spatial and spectral resolution.
We have developed an x-ray microprobe facility utilizing mirror bending techniques that allow white light x-rays from the Advanced Light Source Synchrotron to be focused down to spot sizes of micron spatial dimensions. We have installed a 4 crystal monochromator prior to the micro-focusing mirrors. The monochromator is designed such that it can move out of the way of the input beam, and allows the same micron sized samples to be illuminated with either white or monochromator radiation. Illumination of the sample with white light allows for elemental mapping and Laue x-ray diffraction, while illumination of the sample with monochromatic light allows for elemental mapping, micro-x-ray absorption spectroscopy and microdiffraction. The performance of the system will be described as will some of the initial experiments that cover the various disciplines of Earth, Material and Life Sciences.
Time-dependent x-ray diffraction has been measured from laser-irradiated semiconductor crystals. Laser pulses with 100 fs duration and 800 nm wavelength excite the sample inducing phase transitions. 5 keV x-rays from the Advanced Light Source are diffracted by a sagittally-focusing Si (111) crystal and then by the sample crystal, InSb (111), onto an avalanche photodiode. By detecting individual pulses of synchrotron radiation, which have a duration of 70 ps, the diffracted intensity is observed to decrease because of photoabsorption in a disordered surfaced layer. Rocking curves measured after the laser irradiation show a tail, which results from a strained region caused by expansion of the crystal lattice.
The application of ray deviation calculations based on aberration coefficients for a single optical surface for the design of beamline optical systems is reviewed. A systematic development is presented which allows insight into which aberration may be causing the rays to deviate from perfect focus. A new development allowing analytical calculation of lineshape is presented.
We report here the development of a hard x-ray multilayer grating that has achieved an absolute efficiency of 34% at a wavelength of 1.54A. The W-C multilayer itself has a reflectivity of 57% and
the grating has a 0th order absolute efficiency of 36%. The origin of this extraordinarily high efficiency is that the short period and highly asymmetric structure of the grating combined with its deep grooves allows light to interact with a large number of layer pairs. This increases angular separation of the diffraction orders and reduces the multilayer bandwidth to the point where there is little or no order to order overlap in the grating structure, and hence maximum intensity can be diffracted into a selected order. This paper reports on the development of an optimized multilayer grating and some of its unique characteristics.
Of the many methods used to focus x-rays, the se of mirrors with an elliptical curvature shows the most promise of providing a sub-micron white light focus. Our group has been developing he techniques of controlled bending of mirror substrates in order to produce the desired elliptical shape. We have been successful in producing surfaces with the required microradian slope error tolerances. Details of the bending techniques used, results from laboratory slope error measurements using a Long Trace Profiler and data from the measurement of focus shape using knife edge and imaging methods using x-rays in the 5 - 12 KeV energy range are presented. The development of a white light focusing opens many possibilities in diffraction and spectroscopic studies.
An elliptically bent mirror of total length 1.25 m has been developed at the Advanced Light Source (ALS) for focusing soft x-rays. The mirror is used to produce a small, high flux density illuminated field of view for a Photo-Emission Electron Microscope. The requirement to collect the maximum horizontal aperture with the need to highly demagnify the source leads to a mirror with a wide range of curvatures along the surface. This combined with the need to produce a low slope error surface at a reasonably low cost has required us to develop a mirror based on the controlled bending of a flat substrate. This is an extension of several other mirror projects at the ALS where controlled bending of glass and metal substrates has been used in micro-focusing applications. Those mirrors however are a maximum of 200 mm long, and in this paper we describe the new challenges we have faced and the solutions we have adopted in developing a long and highly elliptical mirror. The mirror described here is manufactured from a low carbon steel (1006) which is capable of good dimensional stability, it is electroless nickel plated for polishing, and is bent into an elliptical shape by the application of unequal couples. We describe the mirror fabrication process, the mechanical details of the bending mechanism and the experimentally measured slope error from an ellipse. The final mirror has an rms roughness of 6 angstroms (rms), a full aperture (1.1 m) slope error of 14 (mu) rad (rms), and a slope error of < 3 (mu) rad when optimized over approximately 2/3 of the required optical length (0.917 m).
The first IR beamline at the advanced light source, Beamline 1.4, is described. The design of the optical and mechanical systems are discussed, including choices and tradeoffs. The initial commissioning of the beamline is reported. The beamline, while designed primarily for IR microscopy and only initially instrumented for microscopy (with a Nicolet interferometer and microscope), will have the potential for surface science experiments at grazing incidence, and time- resolved visible spectroscopy.
The optical design of a varied line-space spectrograph for the multi-channel recording of NEXAFS spectra in a single `snapshot' is proposed. The spectrograph is to be used with a bending magnet source on beamline 7.3.2 at the Advanced Light Source. Approximately 20 volts of spectra are simultaneously imaged across a small square of material sample at each respective K absorption edge of carbon, nitrogen, and oxygen. Photoelectrons emitted from the material sample will be collected by an electron imaging microscope, the view field of which determines the sampling size. The sample also forms the exit slit of the optical system. This dispersive method of NEXAFS data acquisition is three to four orders of magnitude faster than the conventional method of taking data point-to-point using scanning of the grating. The proposed design is presented along with the design method and supporting SHADOW raytrace analysis.
Although x-ray micro-foci can be produced by a variety of diffractive methods, grazing incidence mirrors are the only route to an achromatic focus. In this paper we describe our efforts to produce elliptically shaped mirrors with the very high figure accuracy necessary for producing a micro-focus. The motivation for this work is provided by the need to produce achromatic foci for a range of applications ranging from tunable micro-focus x-ray photoelectron spectroscopy ((mu) -XPS) at soft x-ray energies to micro-focus white beam x-ray diffraction ((mu) -XRD) at hard x-ray energies. We describe the methodology of beam bending, a practical example of a system we have produced for (mu) -XRD, and results demonstrating the production of a surface with micro-radian figure accuracy.
A beamline for high resolution spectroscopy with elliptically polarized X-rays is described. The working energy range is large, from 20 eV to above 1800 eV. The resolving power is on the order of 10,000 at low energies (20 eV - 200 eV) and 6000 at high energies (200 eV - 1800 eV). This is achieved using a variable deviation angle plane grating monochromator. A single grating, with one line density and a varying groove depth, is used to cover the entire energy range. The beamline has been designed to operate with either one or two x-ray beams propagating simultaneously through the monochromator and to the experimental station. Switching between polarizations at rates of 0.1 Hz and slower is accomplished in the single beam mode by alternating the output of the elliptically polarized undulator source between left and right polarization. Fast polarization switching, at rates of 100 - 1000 Hz, is provided in the two beam mode by mechanical chopping between two photon beams, one of which is right circularly polarized, and the other left circularly polarized.
A 2D pixel array image sensor module has been designed for time resolved Protein Crystallography. This smart pixels detector significantly enhances time resolved Laue Protein crystallography by two or three orders of magnitude compared to existing sensors like films or phosphor screens coupled to CCDs. The resolution in time and dynamic range of this type of detector will allow to study the evolution of structural changes that occur within the protein as a function of time. This detector will also considerably accelerate data collection in static Laue or monochromatic crystallography and make better use of the intense beam delivered by synchrotron light sources. The event driven pixel array detectors, based on the column architecture, can provide multiparameter information (energy discrimination, time), with sparse and frameless readout without significant dead time. The prototype module consists of a 16 by 16 pixel diode array bump-bonded to the integrated circuit. Different detector materials (Silicon, CdZnTe) are evaluated. The detection area is 150 by 150 micrometers2 connected to the readout electronics. The individual pixel processor consists of a low-noise amplifier shaper followed by a differential threshold comparator which provides the counting of individual photons with an energy above a programmable threshold. To accommodate the very high rates, above 5 by 108/cm2/s, each pixel processor has a 3 bit pre-scaler which divides the event rate by 8. Overflow from the divider which defines a pseudo fourth bit will generate a readout sequence providing the pixel address. Addresses, generated locally as analog signals, are converted off-chip and used to increment a location in an histogramming memory to generate the computerized image of the Laue diagram.
A beamline for circularly polarized radiation produced by an elliptical wiggler has been designed at the ALS. It covers a broad energy range from 50 eV to 2000 eV. The rigorous theory of grating diffraction efficiency has been used to maximize throughput. This is a challenging optical problem due to the nature of the elliptical wiggler insertion device. The wiggler has a large source size in the vertical and horizontal directions, and the monochromator requires high resolution (small slits), a wide tuning range, and cooling for high heat loads. These problems have been solved by using a variable included angle monochromator with high demagnification onto the entrance slit, aberration correction of the grating for the large vertical aperture, and cooled optics.
Problems of short period multilayer mirrors fabrication are discussed. Results of synthesis of multilayer structures with nanometer period are presented. The shortest period observed is 13 angstroms for W - Si and W - B4C sputtered multilayers. Measurements of near normal incidence reflectivity at (lambda) equals 31 - 32 angstroms are described for W - Sc multilayers with period about 16 angstroms. Measured reflectivity achieves 3.3% and is in good agreement with theoretical model.
The useful flux received in an experiment will depend both on the characteristics of the source and on the characteristics of the experiment. It is therefore necessary when optimizing the design of a synchrotron radiation source to take full account of the experimental requirements and not simply to optimize the integrated flux or brilliance. A method of optimization used for multipole wigglers and bending magnets is described, and applied to a proposed 3 GeV source at Daresbury, DIAMOND, and the proposed 2.1 GeV Swiss Light Source, SLS.
Comparisons between Electromagnetic Theory predictions and measurements are presented for four types of gratings supporting a very high number of diffracted orders. The first type consists of gold coated gratings used in soft X-ray region. The second one is a multilayer grating designed to have a broad reflection band around 0.6 nm wavelength. The third type is a transmission echelle used in the visible and the fourth, an echelette grating for use in the X-ray region. Good agreement between theory and experiment was found in all cases. In the latter case, the groove shape was far from ideal but using the real measured profile in the efficiency calculation good agreement was found even in this extreme situation.
A broadband Rh/C (50/50) multilayer coating was deposited on a blazed reflection grating replica sample. A calculation of possible materials and configurations showed that a 6-layer pair multilayer of rhodium/carbon or a 7 layer of nickel/carbon covered by 2 nm rhodium layer would give a factor of 6-10 increase in reflection efficiency depending on the roughness of the layer interfaces. Measurements with X-rays at wavelengths down to 0.4 nm on a Rh/C multilayer blazed grating combination showed a substantial increase in reflectivity with respect to a gold coated grating for a fixed angle of incidence of 1 deg.
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