Optimized alignment of X-ray mirrors with an automated speckle-based metrology tool.

X-ray mirrors are widely used in beamlines and laboratories as focusing or collimating optics. As well as the highly accurate processes used to fabricate them, optimized alignment of X-ray mirrors also plays an important role in achieving an ideal X-ray beam. Currently, knife-edge scans are the most often used method for aligning X-ray mirrors, which can characterize the focal size and tune the alignment iteratively. However, knife-edge scanning provides only one-dimensional information and this method suffers from being time-consuming and requiring a high-resolution piezo translation stage. Here we describe a straightforward and non-iterative method for mirror alignment by measuring the relationship between the tilt aberration and the misaligned pitch angle, which is retrieved by an at-wavelength metrology technique using a randomly shaped wavefront modulator. Software and a graphical user interface have been developed to automate the alignment process. Combining the user-friendly interface and the flexibility of the at-wavelength metrology technique, we believe the proposed method and software can benefit researchers working at synchrotron facilities and on laboratory sources.

Characterization of a submicro-X-ray fluorescence setup on the B16 beamline at Diamond Light Source.

An X-ray fluorescence setup has been tested on the B16 beamline at the Diamond Light Source synchrotron with two different excitation energies (12.7 and 17 keV). This setup allows the scanning of thin samples (thicknesses up to several micrometers) with a sub-micrometer resolution (beam size of 500 nm × 600 nm determined with a 50 µm Au wire). Sensitivities and detection limits reaching values of 249 counts s-1 fg-1 and 4 ag in 1000 s, respectively (for As Kα excited with 17 keV), are presented in order to demonstrate the capabilities of this setup. Sample measurements of a human bone and a single cell performed at B16 are presented in order to illustrate the suitability of the setup in biological applications.

Mapping of multi-elements during melting and solidification using synchrotron X-rays and pixel-based spectroscopy.

A new synchrotron-based technique for elemental imaging that combines radiography and fluorescence spectroscopy has been developed and applied to study the spatial distribution of Ag, Zr and Mo in an Al alloy during heating and melting to 700, and then re-soldification. For the first time, multi-element distributions have been mapped independently and simultaneously, showing the dissolution of Ag- and Zr-rich particles during melting and the inter-dendritic segregation of Ag during re-solidification. The new technique is shown to have wide potential for metallurgical and materials science applications where the dynamics of elemental re-distribution and segregation in complex alloys is of importance.

Nanofocusing optics for synchrotron radiation made from polycrystalline diamond.

Diamond possesses many extreme properties that make it an ideal material for fabricating nanofocusing x-ray optics. Refractive lenses made from diamond are able to focus x-ray radiation with high efficiency but without compromising the brilliance of the beam. Electron-beam lithography and deep reactive-ion etching of silicon substrates have been used in a transfer-molding technique to fabricate diamond optics with vertical and smooth sidewalls. Latest generation compound refractive lenses have seen an improvement in the quality and uniformity of the optical structures, resulting in an increase in their focusing ability. Synchrotron beamline tests of two recent lens arrays, corresponding to two different diamond morphologies, are described. Focal line-widths down to 210 nm, using a nanocrystalline diamond lens array and a beam energy of E = 11 keV, and 230 nm, using a microcrystalline diamond lens at E = 15 keV, have been measured using the Diamond Light Source Ltd. B16 beamline. This focusing prowess is combined with relatively high transmission through the lenses compared with silicon refractive designs and other diffractive optics.

High efficiency nano-focusing kinoform optics for synchrotron radiation.

Modern synchrotron sources have provided for decades intense beams of photons over a large energy spectrum. The availability of improved optics and detectors has opened up new opportunities for the study of matter at the micrometre and nanometre scale in many disciplines. Whilst exploitation of micro-focused beams occurs almost daily in many beamlines, the production of beams of 100 nm is achieved on few instruments which use specialised optics. Refractive lenses, zone plates, curved mirrors, multilayers, and multilayer Laue lenses, can all focus x-rays to less than 50 nm under strict beam stability conditions. Focusing the synchrotron radiation to beam sizes smaller than 10 nm is considered the ultimate goal for the current decade. Silicon micro-technology has so far provided some of the most advanced x-ray refractive lenses; we report on design and characterisation of a novel silicon kinoform lens that is capable of delivering nano-beams with high efficiency.

High-precision soft x-ray polarimeter at Diamond Light Source.

The development and performance of a high-precision polarimeter for the polarization analysis in the soft x-ray region is presented. This versatile, high-vacuum compatible instrument is supported on a hexapod to simplify the alignment with a resolution less than 5 µrad, and can be moved with its own independent control system easily between different beamlines and synchrotron facilities. The polarimeter can also be used for the characterization of reflection and transmission properties of optical elements. A W/B(4)C multilayer phase retarder was used to characterize the polarization state up to 1200 eV. A fast and accurate alignment procedure was developed, and complete polarization analysis of the APPLE II undulator at 712 eV has been performed.

Application of kinoform lens for X-ray reflectivity analysis.

In this paper the first practical application of kinoform lenses for the X-ray reflectivity characterization of thin layered materials is demonstrated. The focused X-ray beam generated from a kinoform lens, a line of nominal size approximately 50 microm x 2 microm, provides a unique possibility to measure the X-ray reflectivities of thin layered materials in sample scanning mode. Moreover, the small footprint of the X-ray beam, generated on the sample surface at grazing incidence angles, enables one to measure the absolute X-ray reflectivities. This approach has been tested by analyzing a few thin multilayer structures. The advantages achieved over the conventional X-ray reflectivity technique are discussed and demonstrated by measurements.

Structural characterization of thin layered materials using x-ray standing wave enhanced elastic and inelastic scattering measurements.

By measuring the intensities of the x-ray standing wave induced elastic and inelastic x-ray scattering from thin multilayer structures, we show that structural characterizations of the high and low z (atomic number) material layers can be performed independently. The method has been tested by analyzing the structural properties of an Nb/C/Nb trilayer and an Mo/Si periodic multilayer structure. The results of the x-ray scattering measurements have been compared with those obtained using x-ray reflectivity and conventional x-ray standing wave fluorescence techniques. It has been demonstrated that the present approach is especially suitable for studying multilayer structures comprising low atomic number layers, as it eliminates the requirement of a fluorescence signal, which is very weak in the case of low z materials.

Characterization of germanium linear kinoform lenses at Diamond Light Source.

The unprecedented brilliance achieved by third-generation synchrotron sources and the availability of improved optics have opened up new opportunities for the study of materials at the micrometre and nanometre scale. Focusing the synchrotron radiation to smaller and smaller beams is having a huge impact on a wide research area at synchrotrons. The key to the exploitation of the improved sources is the development of novel optics that deliver narrow beams without loss of brilliance and coherence. Several types of synchrotron focusing optics are successfully fabricated using advanced miniaturization techniques. Kinoform refractive lenses are being developed for hard X-ray beamlines, and the first test results at Diamond are discussed in this paper.

Sample preparation for evaluation of detection limits in X-ray fluorescence spectrometry.

The influence of analyte mass concentration on determination of detection limits in X-ray fluorescence spectrometry has been investigated experimentally. Both the total reflection X-ray fluorescence (TXRF) and the conventional energy-dispersive X-ray fluorescence techniques have been used to derive the dependence of analyte mass concentration on the values of detection limits. Results obtained indicate that values of detection limits are optimum, or in other words, they are closer to the true detection limit of the technique, when analyte concentrations are in the range of 10 times of the detection limit.