Atomic layer deposition frequency-multiplied Fresnel zone plates for hard x-rays focusing (original) (raw)

Efficient focusing of 8 keV X-rays with multilayer Fresnel zone plates fabricated by atomic layer deposition and focused ion beam milling

Journal of Synchrotron Radiation, 2013

Fresnel zone plates (FZPs) recently showed significant improvement by focusing soft X-rays down to $ 10 nm. In contrast to soft X-rays, generally a very high aspect ratio FZP is needed for efficient focusing of hard X-rays. Therefore, FZPs had limited success in the hard X-ray range owing to difficulties of manufacturing high-aspect-ratio zone plates using conventional techniques. Here, employing a method of fabrication based on atomic layer deposition (ALD) and focused ion beam (FIB) milling, FZPs with very high aspect ratios were prepared. Such multilayer FZPs with outermost zone widths of 10 and 35 nm and aspect ratios of up to 243 were tested for their focusing properties at 8 keV and shown to focus hard X-rays efficiently. This success was enabled by the outstanding layer quality thanks to ALD. Via the use of FIB for slicing the multilayer structures, desired aspect ratios could be obtained by precisely controlling the thickness. Experimental diffraction efficiencies of multilayer FZPs fabricated via this combination reached up to 15.58% at 8 keV. In addition, scanning transmission X-ray microscopy experiments at 1.5 keV were carried out using one of the multilayer FZPs and resolved a 60 nm feature size. Finally, the prospective of different material combinations with various outermost zone widths at 8 and 17 keV is discussed in the light of the coupled wave theory and the thin-grating approximation. Al 2 O 3 /Ir is outlined as a promising future material candidate for extremely high resolution with a theoretical efficiency of more than 20% for as small an outermost zone width as 10 nm at 17 keV.

Deep reactive ion etching of silicon moulds for the fabrication of diamond x-ray focusing lenses

Journal of Micromechanics and Microengineering, 2013

Diamond is a highly desirable material for use in x-ray optics and instrumentation. However, due to its extreme hardness and resistance to chemical attack, diamond is difficult to form into a structure suitable for x-ray lenses. Refractive lenses are capable of delivering x-ray beams with nanoscale resolution. A moulding technique for the fabrication of diamond lenses is reported. High-quality silicon moulds were made using photolithography and deep reactive ion etching. The study of the etch process conducted to achieve silicon moulds with vertical sidewalls and minimal surface roughness is discussed. Issues experienced when attempting to deposit diamond into a high-aspect-ratio mould by chemical vapour deposition are highlighted. Two generations of lenses have been successfully fabricated using this transfer-moulding approach with significant improvement in the quality and performance of the optics observed in the second iteration. Testing of the diamond x-ray optics on the Diamond Light Source Ltd synchrotron B16 beamline has yielded a line focus of sub-micrometre width.

A planar refractive x-ray lens made of nanocrystalline diamond

Journal of Applied Physics, 2010

Diamond has unique properties which make it the ideal material for use in synchrotron instrumentation. X-ray optics made of diamond are almost transparent, they possess strength, and are subject to very low thermal expansion; therefore they will be able to withstand the powerful beams generated by fourth-generation light sources without compromising brilliance. For this reason, several groups are attempting fabrication of refractive lenses and zone plates made of diamond. Lithography and, in general, microfabrication technology, are the ultimate tools for the innovation of synchrotron focusing optics. We propose to combine modern silicon microtechnology with advanced deposition methods to fabricate nanocrystalline-diamond lenses for third-and fourth-generation synchrotron sources. The fabrication method is described here and microfocusing synchrotron tests are illustrated.

High-efficiency and low-absorption Fresnel compound zone plates for hard X-ray focusing

Design and Microfabrication of Novel X-Ray Optics, 2002

Circular and linear zone plates have been fabricated on the surface of silicon crystals for the energy of 8 keV by electron beam lithography and deep ion plasma etching methods. Various variants of compound zone plates with first, second, third diffraction orders have been made. The zone relief height is about 10 mkm, the outermost zone width of the zone plate is 0.4 mkm. The experimental testing of the zone plates has been conducted on SPring-8 and ESRF synchrotron radiation sources. A focused spot size and diffraction efficiency measured by knife-edge scanning are accordingly 0.5 mkm and 39% for the first order circular zone plate.

Hard X-ray focusing by stacked Fresnel zone plates

2007

Stacking technique was developed in order to increase focusing efficiency of Fresnel zone plates at high energies. Two identical Si chips each of which containing Fresnel zone plates were used for stacking. Alignment of the chips was achieved by on-line observation of the moiré pattern from the two zone plates. The formation of moiré patterns was studied theoretically and experimentally at different experimental conditions. To provide the desired stability Si-chips with zone plates were bonded together with slow solidification speed epoxy glue. Technique of angular alignment in order to compensate a linear displacement in the process of gluing was proposed. Two sets of stacked FZPs were produced and experimentally tested to focus 15 and 50 keV X-rays. Gain in the efficiency by factor 2.5 was demonstrated at 15 keV. Focal spot of 1.8 µm vertically and 14 µm horizontally with 35% efficiency was measured at 50 keV. Forecast for the stacking of nanofocusing Fresnel zone plates was discussed.

Diamond planar refractive lenses for third- and fourth-generation X-ray sources

Journal of Synchrotron Radiation, 2003

The fabrication and testing of planar refractive hard X-ray lenses made from bulk CVD diamond substrates is reported. The lens structures were generated by electron-beam lithography and transferred by reactive-ion etching into the diamond. Various lens designs were fabricated and tested at 12.4 and 17.5 keV photon energy. Ef®ciencies of up to 71% and gains of up to 26 were achieved. A line focus of 3.2 mm (FWHM) was measured. These lenses should be able to withstand the extreme¯ux densities expected at the planned fourth-generation X-ray sources.

Characteristics of chemical vapor deposition diamond films for x-ray mask substrates

Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, 1999

In this article we summarize the development and characterization of chemical vapor deposition diamond films used for x-ray mask substrates. Good control of the deposition parameters governing film stress and film thickness has been achieved, and optical transmission greater than 40% has been demonstrated. Novel polishing techniques were employed to reduce the diamond surface roughness to below 3.0 nm Ra. The crystal structure of the diamond material, determined by Raman spectroscopy, transmission electron microscopy and electron diffraction analysis, is polycrystalline, with grain sizes of approximately 10 nm. Accelerated radiation damage testing indicates a correlation between hydrogen content in the films and the degree of distortion. X-ray masks using diamond membranes have been successfully fabricated to provide early learning of image-size and image-placement performance.

Nanofocusing of hard X-ray free electron laser pulses using diamond based Fresnel zone plates

2011

A growing number of X-ray sources based on the free-electron laser (XFEL) principle are presently under construction or have recently started operation. The intense, ultrashort pulses of these sources will enable new insights in many different fields of science. A key problem is to provide x-ray optical elements capable of collecting the largest possible fraction of the radiation and to focus into the smallest possible focus. As a key step towards this goal, we demonstrate here the first nanofocusing of hard XFEL pulses.

Process design for the manufacturing of soft X-ray gratings in single-crystal diamond by high-energy heavy-ion irradiation

The European Physical Journal Plus

This paper describes in detail a novel manufacturing process for optical gratings suitable for use in the UV and soft X-ray regimes in a single-crystal diamond substrate based on highly focused swift heavy-ion irradiation. This type of grating is extensively used in light source facilities such as synchrotrons or free electron lasers, with ever-increasing demands in terms of thermal loads, depending on beamline operational parameters and architecture. The process proposed in this paper may be a future alternative to current manufacturing techniques, providing the advantage of being applicable to single-crystal diamond substrates, with their unique properties in terms of heat conductivity and radiation hardness. The paper summarizes the physical principle used for the grating patterns produced by swift heavy-ion irradiation and provides full details for the manufacturing process for a specific grating configuration, inspired in one of the beamlines at the ALBA synchrotron light sourc...

High-efficiency Fresnel zone plates for hard X-rays by 100 keV e-beam lithography and electroplating

Journal of Synchrotron Radiation, 2011

The fabrication and characterization of Fresnel zone plates (FZPs) for hard X-ray microscopy applications are reported. High-quality 500 nm-and 1 mmthick Au FZPs with outermost zone widths down to 50 nm and 70 nm, respectively, and with diameters up to 600 mm were fabricated. The diffraction efficiencies of the fabricated FZPs were measured for a wide range of X-ray energies (2.8-13.2 keV) showing excellent values up to 65-75% of the theoretical values, reflecting the good quality of the FZPs. Spatially resolved diffraction efficiency measurements indicate the uniformity of the FZPs and a defect-free structure.