Raymond Conley

11 nm hard X-ray focus from a large-aperture multilayer Laue lens

The focusing performance of a multilayer Laue lens (MLL) with 43.4 μm aperture, 4 nm finest zone width and 4.2 mm focal length at 12 keV was characterized with X-rays using ptychography method. The reconstructed probe shows a full-width-at-half-maximum (FWHM) peak size of 11.2 nm. The obtained X-ray wavefront shows excellent agreement with the dynamical calculations, exhibiting aberrations less than 0.3 wave period, which ensures the MLL capable of producing a diffraction-limited focus while offering a sufficient working distance. This achievement opens up opportunities of incorporating a variety of in-situ experiments into ultra high-resolution X-ray microscopy studies.

Pushing the limits: an instrument for hard X-ray imaging below 20 nm

Hard X-ray microscopy is a prominent tool suitable for nanoscale-resolution non-destructive imaging of various materials used in different areas of science and technology. With an ongoing effort to push the 2D/3D imaging resolution down to 10 nm in the hard X-ray regime, both the fabrication of nano-focusing optics and the stability of the microscope using those optics become extremely challenging. In this work a microscopy system designed and constructed to accommodate multilayer Laue lenses as nanofocusing optics is presented. The developed apparatus has been thoroughly characterized in terms of resolution and stability followed by imaging experiments at a synchrotron facility. Drift rates of ∼2 nm h(-1) accompanied by 13 nm × 33 nm imaging resolution at 11.8 keV are reported.

High-efficiency diffractive x-ray optics from sectioned multilayers

We investigate the diffraction properties of sectioned multilayers in Laue (transmission) geometry, at hard x-ray energies (9.5 and 19.5keV). Two samples are studied, a W∕Si multilayer of 200×(29nm) periods, and a Mo∕Si multilayer of 2020×(7nm) periods, with cross-section depths ranging from 2to17μm. Reflectivities as high as 70% are observed. This exceeds the theoretical limit for standard zone plates operating in the multibeam regime, demonstrating that all of the intensity can be directed into a single diffraction order in small-period structures.

Design and performance of a scanning ptychography microscope

We have designed and constructed a dedicated instrument to perform ptychography measurements and characterization of multilayer Laue lenses nanofocusing optics. The design of the scanning microscope provides stability of components and minimal thermal drifts, requirements for nanometer scale spatial resolution measurements. We performed thorough laboratory characterization of the instrument in terms of resolution and thermal drifts with subsequent measurements at a synchrotron. We have successfully acquired and reconstructed ptychography data yielding 11 nm line focus.

Profile coatings and their applications

We report a method of profile coating to achieve a certain selected thickness profile of a thin film coating using dc magnetron sputtering. In profile coatings, the substrate is passed over a contoured mask at a constant speed to obtain a desired profile along the direction perpendicular to the substrate-moving direction. The shape of the contour depends on the desired profile and the thickness distribution directly above the gun at the substrate level. Si wafers of 4 in. diameter were coated through a 100×152 mm2 aperture on the top of the shield can. The thickness distribution was then obtained using a spectroscopic ellipsometer with computer-controlled X-Y stages. A model has been developed to fit the measured thickness distribution. The relative thickness weightings are then obtained at every point 1 mm apart for the entire open area of the aperture. When the substrate is moving across the shield can during depositions, the film thickness is directly proportional to the length of the opening on the ca...

Efficiency of a multilayer-Laue-lens with a 102 μm aperture

A multilayer-Laue-lens (MLL) comprised of WSi2/Al layers stacked to a full thickness of 102 μm was characterized for its diffraction efficiency and dynamical diffraction properties by x-ray measurements made in the far field. The achieved aperture roughly doubles the previous maximum reported aperture for an MLL, thereby doubling the working distance. Negative and positive first orders were found to have 14.2% and 13.0% efficiencies, respectively. A section thickness of 9.6 μm was determined from Laue-case thickness fringes in the diffraction data. A background gas consisting of 90% Ar and 10% N2 was used for sputtering. This material system was chosen to reduce grown-in stress as the multilayer is deposited. Although some regions of the full MLL exhibited defects, the presently reported results were obtained for a region devoid of defects. The data compare well to dynamical diffraction calculations with Coupled Wave Theory (CWT) which provided confirmation of the optical constants and densities assumed for the CWT calculations.

Film stress studies and the multilayer Laue lens project

A Multilayer Laue Lens (MLL) is a new type of linear zone plate, made by sectioning a planar depth-graded multilayer and used in Laue transmission diffraction geometry, for nanometer-scale focusing of hard x-rays. To produce an MLL, a depth-graded multilayer consisting of thousands of layers with a total thickness of tens of microns is needed. Additionally, the multilayer wafer has to be sectioned and polished to a thickness of ~10 to 25 microns to yield a diffracting grating to focus x-rays. The multilayers must have both low stress and good adhesion to survive the subsequent cutting and polishing processes, as well as sharp interfaces and accurate layer placement. Several partial MLLs using WSi2/Si multilayers with precise zone-plate structures have been successfully fabricated. A W/Si multilayer with the same structure, however, cracked and peeled off from the Si substrate after it was grown. Here we report results of our film stress studies of dc magnetron-sputtered WSi2, W, and Mo thin films and WSi2/Si, W/Si, and Mo/Si multilayers grown on Si(100) substrates. The stress measurements were carried out using a stylus profiler to measure the curvatures of 2-inch-diameter, 0.5-mm-thick Si(100) wafers before and after each coating. The physical origins of the stress and material properties of these systems will be discussed.

Diffraction properties of multilayer Laue lenses with an aperture of 102 µm and WSi₂/Al bilayers.

We report on the characterization of a multilayer Laue lens (MLL) with large acceptance, made of a novel WSi2/Al bilayer system. Fabrication of multilayers with large deposition thickness is required to obtain MLL structures with sufficient apertures capable of accepting the full lateral coherence length of x-rays at typical nanofocusing beamlines. To date, the total deposition thickness has been limited by stress-buildup in the multilayer. We were able to grow WSi2/Al with low grown-in stress, and asses the degree of stress reduction. X-ray diffraction experiments were conducted at beamline 1-BM at the Advanced Photon Source. We used monochromatic x-rays with a photon energy of 12 keV and a bandwidth of ΔE/E=5.4·10(-4). The MLL was grown with parallel layer interfaces, and was designed to have a large focal length of 9.6 mm. The mounted lens was 2.7 mm in width. We found and quantified kinks and bending of sections of the MLL. Sections with bending were found to partly have a systematic progression in the interface angles. We observed kinking in some, but not all, areas. The measurements are compared with dynamic diffraction calculations made with Coupled Wave Theory. Data are plotted showing the diffraction efficiency as a function of the external tilting angle of the entire mounted lens. This way of plotting the data was found to provide an overview into the diffraction properties of the whole lens, and enabled the following layer tilt analyses.

X-ray optics testing beamline 1-BM at the advanced photon source

Beamline 1-BM at the APS has been reconfigured in part for testing of synchrotron optics with both monochromatic and white beams. Operational since 2013, it was reconfigured to accommodate users of the APS as well as users from other DOE facilities. Energies between 6 and 28 keV are available. The beamline was reconfigured to remove two large mirrors and to provide a 100 mm wide monochromatic beam at 54 m from the source. In addition a custom white beam shutter was implemented for topography exposures as short as 65 millisec over the full available horizontal width. Primary agendas include both white beam and monochromatic beam topography, Talbot grating interferometry, and tests of focusing optics. K-B mirrors, MLLs, and FZPs have been characterized. Measurements of the spatial coherence lengths on the beamline were obtained with Talbot interferometry. Topography data has been reported.

WSi2/Si multilayer sectioning by reactive ion etching for multilayer Laue lens fabrication

Reactive ion etching (RIE) has been employed in a wide range of fields such as semiconductor fabrication, MEMS (microelectromechanical systems), and refractive x-ray optics with a large investment put towards the development of deep RIE. Due to the intrinsic differing chemistries related to reactivity, ion bombardment, and passivation of materials, the development of recipes for new materials or material systems can require intense effort and resources. For silicon in particular, methods have been developed to provide reliable anisotropic profiles with good dimensional control and high aspect ratios1,2,3, high etch rates, and excellent material to mask etch selectivity. A multilayer Laue lens4 is an x-ray focusing optic, which is produced by depositing many layers of two materials with differing electron density in a particular stacking sequence where the each layer in the stack satisfies the Fresnel zone plate law. When this stack is sectioned to allow side-illumination with radiation, the diffracted exiting radiation will constructively interfere at the focal point. Since the first MLLs were developed at Argonne in the USA in 20064, there have been published reports of MLL development efforts in Japan5, and, very recently, also in Germany6. The traditional technique for sectioning multilayer Laue lens (MLL) involves mechanical sectioning and polishing7, which is labor intensive and can induce delamination or structure damage and thereby reduce yield. If a non-mechanical technique can be used to section MLL, it may be possible to greatly shorten the fabrication cycle, create more usable optics from the same amount of deposition substrate, and perhaps develop more advanced structures to provide greater stability or flexibility. Plasma etching of high aspect-ratio multilayer structures will also expand the scope for other types of optics fabrication (such as gratings, zone plates, and so-on). However, well-performing reactive ion etching recipes have been developed for only a small number of materials, and even less recipes exist for concurrent etching of more than one element so a fully material specific process needs to be developed. In this paper, sectioning of WSi2/Si multilayers for MLL fabrication using fluorinated gases is investigated. The main goals were to demonstrate the feasibility of this technique, achievement of high anisotropy, adequate sidewall roughness control and high etching rates. We note that this development for MLL sidewalls should be distinguished from work on improving aspect ratios in traditional Fresnel zone plates. Aspect ratios for MLL sidewalls are not similarly constrained.