Sub-nanometre quality X-ray mirrors created using ion beam figuring.

Ion beam figuring (IBF) is a powerful technique for figure correction of X-ray mirrors to a high accuracy. Here, recent technical advancements in the IBF instrument developed at Diamond Light Source are presented and experimental results for figuring of X-ray mirrors are given. The IBF system is equipped with a stable DC gridded ion source (120 mm diameter), a four-axis motion stage to manipulate the optic, a Faraday cup to monitor the ion-beam current, and a camera for alignment. A novel laser speckle angular measurement instrument also provides on-board metrology. To demonstrate the IBF system's capabilities, two silicon X-ray mirrors were processed. For 1D correction, a height error of 0.08 nm r.m.s. and a slope error of 44 nrad r.m.s. were achieved. For 2D correction over a 67 mm × 17 mm clear aperture, a height error of 0.8 nm r.m.s. and a slope error of 230 nrad r.m.s. were obtained. For the 1D case, this optical quality is comparable with the highest-grade, commercially available, X-ray optics.

Ion beam figuring for X-ray mirrors: history, state-of-the-art and future prospects.

Synchrotron light sources require X-ray optics with extremely demanding accuracy for the surface profile, with less than 100 nrad slope errors and sub-nanometre height errors. Such errors are challenging to achieve for aspheres using traditional polishing methods. However, post-polishing error correction can be performed using techniques such as ion beam figuring (IBF) to improve optics to the desired quality. This work presents a brief overview of the history of IBF, introduces some of the challenges for obtaining such demanding figure errors, and highlights the work done at several in-house IBF facilities at synchrotron light sources worldwide to obtain state-of-the-art optical quality.

Correcting retrace and system imaging errors to achieve nanometer accuracy in full aperture, single-shot Fizeau interferometry.

X-ray mirrors with single-digit nanometer height errors are required to preserve the quality of ultra-intense photon beams produced at synchrotron or free electron laser sources. To fabricate suitable X-ray mirrors, accurate metrology data is needed for deterministic polishing machines. Fizeau phase-shifting interferometers are optimized to achieve accurate results under nulled conditions. However, for curved or aspheric mirrors, a limited choice of reference optic often necessitates measurement under non-nulled conditions, which can introduce retrace error. Using experimental measurements of a multi-tilted calibration mirror, we have developed an empirical model of Fizeau retrace error, based on Zernike polynomial fitting. We demonstrate that the model is in good agreement with measurements of ultra-high quality, weakly-curved X-ray mirrors with sags of only a few tens of microns. Removing the predicted retrace error improves the measurement accuracy for full aperture, single shot, Fizeau interferometry to < 2 nm RMS.

Real-time spatial characterization of micrometer-sized X-ray free-electron laser beams focused by bendable mirrors.

A real-time and accurate characterization of the X-ray beam size is essential to enable a large variety of different experiments at free-electron laser facilities. Typically, ablative imprints are employed to determine shape and size of µm-focused X-ray beams. The high accuracy of this state-of-the-art method comes at the expense of the time required to perform an ex-situ image analysis. In contrast, diffraction at a curved grating with suitably varying period and orientation forms a magnified image of the X-ray beam, which can be recorded by a 2D pixelated detector providing beam size and pointing jitter in real time. In this manuscript, we compare results obtained with both techniques, address their advantages and limitations, and demonstrate their excellent agreement. We present an extensive characterization of the FEL beam focused to ≈1 µm by two Kirkpatrick-Baez (KB) mirrors, along with optical metrology slope profiles demonstrating their exceptionally high quality. This work provides a systematic and comprehensive study of the accuracy provided by curved gratings in real-time imaging of X-ray beams at a free-electron laser facility. It is applied here to soft X-rays and can be extended to the hard X-ray range. Furthermore, curved gratings, in combination with a suitable detector, can provide spatial properties of µm-focused X-ray beams at MHz repetition rate.

I21: an advanced high-resolution resonant inelastic X-ray scattering beamline at Diamond Light Source.

The I21 beamline at Diamond Light Source is dedicated to advanced resonant inelastic X-ray scattering (RIXS) for probing charge, orbital, spin and lattice excitations in materials across condensed matter physics, applied sciences and chemistry. Both the beamline and the RIXS spectrometer employ divergent variable-line-spacing gratings covering a broad energy range of 280-3000 eV. A combined energy resolution of ∼35 meV (16 meV) is readily achieved at 930 eV (530 eV) owing to the optimized optics and the mechanics. Considerable efforts have been paid to the design of the entire beamline, particularly the implementation of the collection mirrors, to maximize the X-ray photon throughput. The continuous rotation of the spectrometer over 150° under ultra high vacuum and a cryogenic manipulator with six degrees of freedom allow accurate mappings of low-energy excitations from solid state materials in momentum space. Most importantly, the facility features a unique combination of the high energy resolution and the high photon throughput vital for advanced RIXS applications. Together with its stability and user friendliness, I21 has become one of the most sought after RIXS beamlines in the world.

1 m long multilayer-coated deformable piezoelectric bimorph mirror for adjustable focusing of high-energy X-rays.

The Diamond Light Source (DLS) beamline I15-1 measures atomic pair distribution functions (PDF) using scattering of 40-80 keV X-rays. A unique focusing element was needed to condense these X-rays from an initial large cross section (11.0 mm H × 4.2 mm V) into a required spot size of FWHM ≈680 µm (H) × 20 µm (V) at a variable position between the sample and the detector. The large numerical aperture is achieved by coating a silicon substrate over 1 m long with three multilayer stripes of Bragg angle 4.2 mrad. One stripe selects X-rays of each energy 40.0, 65.4, and 76.6 keV. Sixteen piezoelectric bimorph actuators attached to the sides of the mirror substrate adjusted the reflecting surface's shape. Focal spots of vertical width < 15 µm were obtained at three positions over a 0.92 m range, with fast, easy switching from one focal position to another. Minimized root mean square slope errors were close to 0.5 µrad after subtraction of a uniform curvature. Reflectivity curves taken along each stripe showed consistent high peaks with generally small angular variation of peak positions. This is the first application of a 1 m long multilayer-coated bimorph mirror at a synchrotron beamline. Data collected with its help on a slice of a lithium ion battery's cathode are presented.

Application of interference fits on cylindrical monochromator crystals to overcome clamping and cooling deformations.

In order to provide adequate cryogenic cooling of both existing and next-generation crystal monochromators, a new approach to produce an optimum thermal interface between the first crystal and its copper heat exchanger is proposed. This will ensure that the increased heat load deposited by higher X-ray powers can be properly dissipated. Utilizing a cylindrical silicon crystal, a tubular copper heat exchanger and by exploiting the differing thermal and mechanical properties of the two, a very good thermal interface was achieved at liquid-nitrogen temperatures. The surface flatness of the diffracting plane at one end of the cylindrical crystal was measured at room temperature while unconstrained. The crystal was then placed into the copper heat exchanger, a slide fit at room temperature, and then cooled to liquid-nitrogen temperature. At -200°C the slide fit became an interference fit. This room-temperature `loose' fit was modelled using finite-element analysis to obtain the desired fit at cryogenic temperatures by prescribing the fit at room temperature. Under these conditions, the diffraction surface was measured for distortion due to thermal and mechanical clamping forces. The total deformation was measured to be 30 nm, an order of magnitude improvement over deformation caused by cooling alone with the original side-clamped design this concept method is set to replace. This new methodology also has the advantage that it is repeatable and does not require macro-scale tools to acquire a nanometre-accuracy mounting.

High-speed adaptive optics using bimorph deformable x-ray mirrors.

Recently, the dynamic performance of piezo-electric deformable "bimorph" mirrors for synchrotron radiation and X-ray free electron laser sources has been characterized and significantly improved. This innovation enables high intensity X-ray beams to be rapidly focused or defocused to either match to the size of the sample under test or to select different sized regions of interest in larger samples. In this paper, we extend these results by monitoring a bimorph mirror using a combination of ex situ metrology instruments. Comparison between results from the Diamond-NOM (Nanometre Optical Metrology) slope profiler, a Fizeau interferometer, and Zygo ZPSTM distance measuring probes shows that bimorph X-ray mirrors can reliably and accurately be driven at 1 Hz using advanced features recently added to the high voltage (HV), bipolar "HV-Adaptos" power supply from CAEN.

Dynamic adaptive X-ray optics. Part I. Time-resolved optical metrology investigation of the bending behaviour of piezoelectric bimorph deformable X-ray mirrors.

Piezoelectric bimorph deformable mirrors (`bimorphs') are routinely used on many synchrotron and free-electron laser beamlines to provide active variation in the size and shape of the X-ray beam. However, the time-domain potential of such optics has never been fully exploited. For the first time, the fast dynamic bending response of bimorphs is investigated here using Fizeau interferometry. Automated scripts for acquisition and analysis were developed to collect Fizeau data at a rate of 0.1 Hz to record dynamic changes in the optical surface as voltages were applied to the electrodes of the piezoelectric actuators. It is demonstrated that residual drift in the tangential radius of curvature of a bimorph can be significantly reduced using enhanced opto-mechanical holders and a fast programmable high-voltage power supply. Further improvements are achieved by applying small opposing voltages to compensate for piezoelectric creep. The present study shows that bimorphs can truly be used as high-speed adaptive optics for the X-ray domain, even without closed-loop feedback correction. This opens the possibility for relatively simple real-time tuning of the profile of X-ray bimorphs. Part II of this study [Alcock, Nistea, Signorato, Owen, Axford, Sutter, Foster & Sawhney (2019), J. Synchrotron Rad. 26, 45-51] builds upon these results and demonstrates how bimorphs can rapidly provide customisable sizes and shapes of synchrotron X-ray beams, specifically tailored to suit the experimental samples being investigated.

Dynamic adaptive X-ray optics. Part II. High-speed piezoelectric bimorph deformable Kirkpatrick-Baez mirrors for rapid variation of the 2D size and shape of X-ray beams.

The tangential curvature of actively bent X-ray mirrors at synchrotron radiation and X-ray free-electron laser (XFEL) facilities is typically only changed every few hours or even days. This operation can take tens of minutes for active optics with multiple bending actuators and often requires expert guidance using in situ monitoring devices. Hence, the dynamic performance of active X-ray optics for synchrotron beamlines has historically not been exploited. This is in stark contrast to many other scientific fields. However, many areas of synchrotron radiation and XFEL science, including macromolecular crystallography, could greatly benefit from the ability to change the size and shape of the X-ray beam rapidly and continuously. The advantages of this innovative approach are twofold: a large reduction in the dead time required to change the size of the X-ray beam for different-sized samples and the possibility of making multiple changes to the beam during the measurement of a single sample. In the preceding paper [Part I; Alcock, Nistea, Signorato & Sawhney (2019), J. Synchrotron Rad. 26, 36-44], which accompanies this article, high-speed visible-light Fizeau interferometry was used to identify the factors which influence the dynamic bending behaviour of piezoelectric bimorph deformable X-ray mirrors. Building upon this ex situ metrology study, provided here is the first synchrotron radiation beamline implementation of high-speed adaptive X-ray optics using two bimorphs operating as a Kirkpatrick-Baez pair. With optimized substrates, novel opto-mechanical holders and a next-generation high-voltage power supply, the size of an X-ray beam was rapidly and repeatedly switched in <10 s. Of equal importance, it is also shown that compensation of piezoelectric creep ensures that the X-ray beam size remains stable for more than 1 h after making a major change. The era of high-speed adaptive X-ray optics for synchrotron radiation and XFEL beamlines has begun.

In situ beamline analysis and correction of active optics. Erratum.

A correction to one of the equations in the paper by Sutter et al. (2012). [J. Synchrotron Rad. 19, 960-968] is made.

Long, elliptically bent, active X-ray mirrors with slope errors <200†nrad.

Actively bent X-ray mirrors are important components of many synchrotron and X-ray free-electron laser beamlines. A high-quality optical surface and good bending performance are essential to ensure that the X-ray beam is accurately focused. Two elliptically bent X-ray mirror systems from FMB Oxford were characterized in the optical metrology laboratory at Diamond Light Source. A comparison of Diamond-NOM slope profilometry and finite-element analysis is presented to investigate how the 900 mm-long mirrors sag under gravity, and how this deformation can be adequately compensated using a single, spring-loaded compensator. It is shown that two independent mechanical actuators can accurately bend the trapezoidal substrates to a range of elliptical profiles. State-of-the-art residual slope errors of <200 nrad r.m.s. are achieved over the entire elliptical bending range. High levels of bending repeatability (ΔR/R = 0.085% and 0.156% r.m.s. for the two bending directions) and stability over 24 h (ΔR/R = 0.07% r.m.s.) provide reliable beamline performance.

Creating flat-top X-ray beams by applying surface profiles of alternating curvature to deformable piezo bimorph mirrors.

Beam shaping is becoming increasingly important for synchrotron X-ray applications. Although routine for visible light lasers, this is challenging for X-rays due to the limited source coherence and extreme optical tolerances required for the shaping mirrors. In deliberate defocusing, even surface errors <5 nm r.m.s. introduce damagingly large striations into the reflected beam. To counteract such problems, surface modifications with alternating concave and convex curvature on equal segments were polished onto the surface of non-active mirrors of fixed curvature. Such optics are useful for providing a fixed size of X-ray beam, but do not provide the adaptability required by many experiments. In contrast, deformable piezo bimorph mirrors permit a continuous range of X-ray beam sizes and shapes. A new theory is developed for applying non-periodic modifications of alternating curvature to optical surfaces. The position and length of the segments may be freely chosen. For the first time, surface modifications of alternating curvature are applied to bimorph mirrors to generate non-Gaussian X-ray beam profiles of specified width. The new theory's freedom is exploited to choose the segments to match the polishing errors of medium wavelength (>10 mm) and the piezos' influence on the mirror's figure. Five- and seven-segment modifications of alternating curvature are calculated and verified by visible light and X-ray metrology. The latter yields beam profiles with less striation than those made by defocusing. Remaining beam striations are explained by applying geometrical optics to the deviations from the ideal surface modifications of alternating curvature.

Nano-metrology: The art of measuring X-ray mirrors with slope errors <100 nrad.

We present a comprehensive investigation of the systematic and random errors of the nano-metrology instruments used to characterize synchrotron X-ray optics at Diamond Light Source. With experimental skill and careful analysis, we show that these instruments used in combination are capable of measuring state-of-the-art X-ray mirrors. Examples are provided of how Diamond metrology data have helped to achieve slope errors of <100 nrad for optical systems installed on synchrotron beamlines, including: iterative correction of substrates using ion beam figuring and optimal clamping of monochromator grating blanks in their holders. Simulations demonstrate how random noise from the Diamond-NOM's autocollimator adds into the overall measured value of the mirror's slope error, and thus predict how many averaged scans are required to accurately characterize different grades of mirror.

In vacuo X-ray data collection from graphene-wrapped protein crystals.

The measurement of diffraction data from macromolecular crystal samples held in vacuo holds the promise of a very low X-ray background and zero absorption of incident and scattered beams, leading to better data and the potential for accessing very long X-ray wavelengths (>3 Å) for native sulfur phasing. Maintaining the hydration of protein crystals under vacuum is achieved by the use of liquid jets, as with serial data collection at free-electron lasers, or is side-stepped by cryocooling the samples, as implemented at new synchrotron beamlines. Graphene has been shown to protect crystals from dehydration by creating an extremely thin layer that is impermeable to any exchanges with the environment. Furthermore, owing to its hydrophobicity, most of the aqueous solution surrounding the crystal is excluded during sample preparation, thus eliminating most of the background caused by liquid. Here, it is shown that high-quality data can be recorded at room temperature from graphene-wrapped protein crystals in a rough vacuum. Furthermore, it was observed that graphene protects crystals exposed to different relative humidities and a chemically harsh environment.

A novel instrument for generating angular increments of 1 nanoradian.

Accurate generation of small angles is of vital importance for calibrating angle-based metrology instruments used in a broad spectrum of industries including mechatronics, nano-positioning, and optic fabrication. We present a novel, piezo-driven, flexure device capable of reliably generating micro- and nanoradian angles. Unlike many such instruments, Diamond Light Source's nano-angle generator (Diamond-NANGO) does not rely on two separate actuators or rotation stages to provide coarse and fine motion. Instead, a single Physik Instrumente NEXLINE "PiezoWalk" actuator provides millimetres of travel with nanometre resolution. A cartwheel flexure efficiently converts displacement from the linear actuator into rotary motion with minimal parasitic errors. Rotation of the flexure is directly measured via a Magnescale "Laserscale" angle encoder. Closed-loop operation of the PiezoWalk actuator, using high-speed feedback from the angle encoder, ensures that the Diamond-NANGO's output drifts by only ∼0.3 nrad rms over ∼30 min. We show that the Diamond-NANGO can reliably move with unprecedented 1 nrad (∼57 ndeg) angular increments over a range of >7000 µrad. An autocollimator, interferometer, and capacitive displacement sensor are used to independently confirm the Diamond-NANGO's performance by simultaneously measuring the rotation of a reflective cube.

Characterization of a next-generation piezo bimorph X-ray mirror for synchrotron beamlines.

Piezo bimorph mirrors are versatile active optics used on many synchrotron beamlines. However, many bimorphs suffer from the `junction effect': a periodic deformation of the optical surface which causes major aberrations to the reflected X-ray beam. This effect is linked to the construction of such mirrors, where piezo ceramics are glued directly below the thin optical substrate. In order to address this problem, a next-generation bimorph with piezos bonded to the side faces of a monolithic substrate was developed at Thales-SESO and optimized at Diamond Light Source. Using metrology feedback from the Diamond-NOM, the optical slope error was reduced to ∼ 0.5 µrad r.m.s. for a range of ellipses. To maximize usability, a novel holder was built to accommodate the substrate in any orientation. When replacing a first-generation bimorph on a synchrotron beamline, the new mirror significantly improved the size and shape of the reflected X-ray beam. Most importantly, there was no evidence of the junction effect even after eight months of continuous beamline usage. It is hoped that this new design will reinvigorate the use of active bimorph optics at synchrotron and free-electron laser facilities to manipulate and correct X-ray wavefronts.

Fast optimization of a bimorph mirror using x-ray grating interferometry.

An x-ray grating interferometer was employed for in situ optimization of an x-ray bimorph mirror. Unlike many other at-wavelength techniques, only a single interferogram image, captured out of the focal plane, is required, enabling the optical surface to be quickly optimized. Moiré fringe analysis was used to calculate the wavefront slope error, which is proportional to the mirror's slope error. Using feedback from grating interferometry, the slope error of a bimorph mirror was reduced to <200 nrad (rms) in only two iterations. This technique has the potential to create photon beams with spatially homogeneous intensities for use in synchrotron and free electron laser beam lines.

At-wavelength metrology of hard X-ray mirror using near field speckle.

We present a method to measure the surface profile of hard X-ray reflective optics with nanometer height accuracy and sub-millimetre lateral resolution. The technique uses X-ray near-field speckle, generated by a scattering membrane translated using a piezo motor, to infer the deflection of X-rays from the surface. The method provides a nano-radian order accuracy on the mirror slopes in both the tangential and sagittal directions. As a demonstration, a pair of focusing mirrors mounted in a Kirkpatrick-Baez (KB) configuration were characterized and the results were in good agreement with offline metrology data. It is hoped that the new technique will provide feedback to optic manufacturers to improve mirror fabrication and be useful for the online optimization of active, nano-focusing mirrors on modern synchrotron beamlines.

Bioactive films produced from self-assembling peptide amphiphiles as versatile substrates for tuning cell adhesion and tissue architecture in serum-free conditions.

The development of versatile bioactive surfaces able to emulate in vivo conditions is of enormous importance to the future of cell and tissue therapy. Tuning cell behaviour on two-dimensional surfaces so that the cells perform as if they were in a natural three-dimensional tissue represents a significant challenge, but one that must be met if the early promise of cell and tissue therapy is to be fully realised. Due to the inherent complexities involved in the manufacture of biomimetic three-dimensional substrates, the scaling up of engineered tissue-based therapies may be simpler if based upon proven two-dimensional culture systems. In this work, we developed new coating materials composed of the self-assembling peptide amphiphiles (PAs) C16G3RGD (RGD) and C16G3RGDS (RGDS) shown to control cell adhesion and tissue architecture while avoiding the use of serum. When mixed with the C16ETTES diluent PA at 13 : 87 (mol mol-1) ratio at 1.25 × 10-3 M, the bioactive PAs were shown to support optimal adhesion, maximal proliferation, and prolonged viability of human corneal stromal fibroblasts (hCSFs), while improving the cell phenotype. These PAs also provided stable adhesive coatings on highly-hydrophobic surfaces composed of striated polytetrafluoroethylene (PTFE), significantly enhancing proliferation of aligned cells and increasing the complexity of the produced tissue. The thickness and structure of this highly-organised tissue were similar to those observed in vivo, comprising aligned newly-deposited extracellular matrix. As such, the developed coatings can constitute a versatile biomaterial for applications in cell biology, tissue engineering, and regenerative medicine requiring serum-free conditions.