ABSTRACT
A new design for a double-sided high-pressure diamond anvil cell laser heating set-up is described. The prototype is deployed at beamline 12.2.2 of the Advanced Light Source at Lawrence Berkeley National Lab. Our compact design features shortened mechanical lever arms, which results in more stable imaging optics, and thus more user friendly and more reliable temperature measurements based on pyrometry. A modification of the peak scaling method was implemented for pyrometry, including an iterative method to determine the absolute peak temperature, thus allowing for quasi-real time temperature mapping of the actual hotspot within a laser-heated diamond anvil cell without any assumptions on shape, size, and symmetry of the hotspot and without any assumptions to the relationship between fitted temperature and peak temperature. This is important since we show that the relationship between peak temperature and temperature obtained by fitting the Planck function against the thermal emission spectrum averaged over the entire hotspot is not constant but depends on variable fitting parameters (in particular, the size and position of the fitting window). The accuracy of the method is confirmed through measuring melting points of metal wires at ambient pressure. Having absolute temperature maps in real time allows for more differentiated analyses of laser heating experiments. We present such an example of the pressure variations within a heated hotspot of AgI at a loaded base pressure of 3.8 GPa.
ABSTRACT
Over the past decade, the advances in grating-based soft X-ray spectrometers have revolutionized the soft X-ray spectroscopies in materials research. However, these novel spectrometers are mostly dedicated designs, which cannot be easily adopted for applications with diverging demands. Here we present a versatile spectrometer design concept based on the Hettrick-Underwood optical scheme that uses modular mechanical components. The spectrometer's optics chamber can be used with gratings operated in either inside or outside orders, and the detector assembly can be reconfigured accordingly. The spectrometer can be designed to have high spectral resolution, exceeding 10 000 resolving power when using small source (â¼1µm) and detector pixels (â¼5µm) with high line density gratings (â¼3000 lines/mm), or high throughput at moderate resolution. We report two such spectrometers with slightly different design goals and optical parameters in this paper. We show that the spectrometer with high throughput and large energy window is particularly useful for studying the sustainable energy materials. We demonstrate that the extensive resonant inelastic X-ray scattering (RIXS) map of battery cathode material LiNi1/3Co1/3Mn1/3O2 can be produced in few hours using such a spectrometer. Unlike analyzing only a handful of RIXS spectra taken at selected excitation photon energies across the elemental absorption edges to determine various spectral features like the localized dd excitations and non-resonant fluorescence emissions, these features can be easily identified in the RIXS maps. Studying such RIXS maps could reveal novel transition metal redox in battery compounds that are sometimes hard to be unambiguously identified in X-ray absorption and emission spectra. We propose that this modular spectrometer design can serve as the platform for further customization to meet specific scientific demands.
ABSTRACT
The Advanced Light Source (ALS) beamline (BL) 10.3.2 is an apparatus for X-ray microprobe spectroscopy and diffraction experiments, operating in the energy range 2.4-17â keV. The performance of the beamline, namely the spatial and energy resolutions of the measurements, depends significantly on the collimation quality of light incident on the monochromator. In the BL 10.3.2 end-station, the synchrotron source is imaged 1:1 onto a set of roll slits which form a virtual source. The light from this source is collimated in the vertical direction by a bendable parabolic cylinder mirror. Details are presented of the mirror design, which allows for precision assembly, alignment and shaping of the mirror, as well as for extending of the mirror operating lifetime by a factor of â¼10. Assembly, mirror optimal shaping and preliminary alignment were performed ex situ in the ALS X-ray Optics Laboratory (XROL). Using an original method for optimal ex situ characterization and setting of bendable X-ray optics developed at the XROL, a root-mean-square (RMS) residual surface slope error of 0.31â µrad with respect to the desired parabola, and an RMS residual height error of less than 3â nm were achieved. Once in place at the beamline, deviations from the designed optical geometry (e.g. due to the tolerances for setting the distance to the virtual source, the grazing incidence angle, the transverse position) and/or mirror shape (e.g. due to a heat load deformation) may appear. Due to the errors, on installation the energy spread from the monochromator is typically a few electron-volts. Here, a new technique developed and successfully implemented for at-wavelength (in situ) fine optimal tuning of the mirror, enabling us to reduce the collimation-induced energy spread to â¼0.05â eV, is described.
ABSTRACT
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.
ABSTRACT
A new facility for high-pressure diffraction and spectroscopy using diamond anvil high-pressure cells has been built at the Advanced Light Source on beamline 12.2.2. This beamline benefits from the hard X-radiation generated by a 6 T superconducting bending magnet (superbend). Useful X-ray flux is available between 5 keV and 35 keV. The radiation is transferred from the superbend to the experimental enclosure by the brightness-preserving optics of the beamline. These optics are comprised of a plane parabola collimating mirror, followed by a Kohzu monochromator vessel with Si(111) crystals (E/DeltaE approximately equal 7000) and W/B4C multilayers (E/DeltaE approximately equal 100), and then a toroidal focusing mirror with variable focusing distance. The experimental enclosure contains an automated beam-positioning system, a set of slits, ion chambers, the sample positioning goniometry and area detector (CCD or image-plate detector). Future developments aim at the installation of a second endstation dedicated to in situ laser heating and a dedicated high-pressure single-crystal station, applying both monochromatic and polychromatic techniques.
ABSTRACT
At the Advanced Light Source, three protein crystallography beamlines have been built that use as a source one of the three 6 T single-pole superconducting bending magnets (superbends) that were recently installed in the ring. The use of such single-pole superconducting bend magnets enables the development of a hard X-ray program on a relatively low-energy 1.9 GeV ring without taking up insertion-device straight sections. The source is of relatively low power but, owing to the small electron beam emittance, it has high brightness. X-ray optics are required to preserve the brightness and to match the illumination requirements for protein crystallography. This was achieved by means of a collimating premirror bent to a plane parabola, a double-crystal monochromator followed by a toroidal mirror that focuses in the horizontal direction with a 2:1 demagnification. This optical arrangement partially balances aberrations from the collimating and toroidal mirrors such that a tight focused spot size is achieved. The optical properties of the beamline are an excellent match to those required by the small protein crystals that are typically measured. The design and performance of these new beamlines are described.