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Although diffractive optics have played a major role in nanoscale soft X-ray imaging, high-resolution and high-efficiency diffractive optics have largely been unavailable for hard X-rays where many scientific, technological and biomedical applications exist. This is owing to the long-standing challenge of fabricating ultra-high aspect ratio high-resolution dense nanostructures. Here we report significant progress in ultra-high aspect ratio nanofabrication of high-resolution, dense silicon nanostructures using vertical directionality controlled metal-assisted chemical etching. The resulting structures have very smooth sidewalls and can be used to pattern arbitrary features, not limited to linear or circular. We focus on the application of X-ray zone plate fabrication for high-efficiency, high-resolution diffractive optics, and demonstrate the process with linear, circular, and spiral zone plates. X-ray measurements demonstrate high efficiency in the critical outer layers. This method has broad applications including patterning for thermoelectric materials, battery anodes and sensors among others.

/pdf/ultra-high-aspect-ratio-high-resolution-nanofabrication-for-3s66vxje08.pdf

Ultra-high aspect ratio high-resolution nanofabrication for hard X-ray diffractive optics.

Multilayer Laue lens (MLL) is a new class of x-ray optics that offer great promise for achieving nanometre-level spatial resolution by focusing hard x-rays. Fabricating an MLL via thin-film deposition provides the means to achieve a linear Fresnel-zone plate structure with zone widths below 1?nm, while retaining a virtually limitless aspect ratio. Despite its similarity to the Fresnel-zone plate, MLL exhibits categorically distinctive focusing properties and their fabrication comes with a wide array of challenges. This article provides a comprehensive review of advances in MLLs, and includes extensive theoretical modelling on focusing performance, discussion on fabrication challenges, their current capabilities and notable results from x-ray focusing experiments.

https://iopscience.iop.org/article/10.1088/0022-3727/47/26/263001/pdf

Hard x-ray nanofocusing by multilayer Laue lenses

Characterizing the chemistry and magnetism of magnetotactic bacteria (MTB) is an important aspect of understanding the biomineralization mechanism and function of the chains of magnetosomes (Fe3O4 nanoparticles) found in such species. Images and X-ray absorption spectra (XAS) of magnetosomes extracted from, and magnetosomes in, whole Magnetovibrio blakemorei strain MV-1 cells have been recorded using soft X-ray ptychography at the Fe 2p edge. A spatial resolution of 7 nm is demonstrated. Precursor-like and immature magnetosome phases in a whole MV-1 cell were visualized, and their Fe 2p spectra were measured. Based on these results, a model for the pathway of magnetosome biomineralization for MV-1 is proposed. Fe 2p X-ray magnetic circular dichroism (XMCD) spectra have been derived from ptychography image sequences recorded using left and right circular polarization. The shape of the XAS and XMCD signals in the ptychographic absorption spectra of both sample types is identical to the shape and signals measured with conventional bright-field scanning transmission X-ray microscope. A weaker and inverted XMCD signal was observed in the ptychographic phase spectra of the extracted magnetosomes. The XMCD ptychographic phase spectrum of the intracellular magnetosomes differed from the ptychographic phase spectrum of the extracted magnetosomes. These results demonstrate that spectro-ptychography offers a superior means of characterizing the chemical and magnetic properties of MTB at the individual magnetosome level.

https://www.pnas.org/content/pnas/113/51/E8219.full.pdf

Measuring spectroscopy and magnetism of extracted and intracellular magnetosomes using soft X-ray ptychography

Patterning with a focused ion beam (FIB) is an extremely versatile fabrication process that can be used to create microscale and nanoscale designs on the surface of practically any solid sample material. Based on the type of ion-sample interaction utilized, FIB-based manufacturing can be both subtractive and additive, even in the same processing step. Indeed, the capability of easily creating three-dimensional patterns and shaping objects by milling and deposition is probably the most recognized feature of ion beam lithography (IBL) and micromachining. However, there exist several other techniques, such as ion implantation- and ion damage-based patterning and surface functionalization types of processes that have emerged as valuable additions to the nanofabrication toolkit and that are less widely known. While fabrication throughput, in general, is arguably low due to the serial nature of the direct-writing process, speed is not necessarily a problem in these IBL applications that work with small ion doses. Here we provide a comprehensive review of ion beam lithography in general and a practical guide to the individual IBL techniques developed to date. Special attention is given to applications in nanofabrication.

/pdf/direct-write-ion-beam-lithography-3z1y8by41a.pdf

Direct-Write Ion Beam Lithography

http://xrm.phys.northwestern.edu/research/pdf_papers/2011/mayer_ultramic_2011.pdf

Multilayer Fresnel zone plate for soft X-ray microscopy resolves sub-39 nm structures

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. Al2O3/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.

/pdf/efficient-focusing-of-8-kev-x-rays-with-multilayer-fresnel-1e77t0oouk.pdf

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

X-ray microscopy is a successful technique with applications in several key fields. Fresnel zone plates (FZPs) have been the optical elements driving its success, especially in the soft X-ray range. However, focusing of hard X-rays via FZPs remains a challenge. It is demonstrated here, that two multilayer type FZPs, delivered from the same multilayer deposit, focus both hard and soft X-rays with high fidelity. The results prove that these lenses can achieve at least 21 nm half-pitch resolution at 1.2 keV demonstrated by direct imaging, and sub-30 nm FWHM (full-pitch) resolution at 7.9 keV, deduced from autocorrelation analysis. Reported FZPs had more than 10% diffraction efficiency near 1.5 keV.

Multilayer Fresnel zone plates for high energy radiation resolve 21 nm features at 1.2 keV

Ion beam lithography for direct patterning of high accuracy large area X-ray elements in gold on membranes

A method of producing a Fresnel zone plate (15) comprising: making available a substrate (1, 4, 7) which is rotationally symmetrical with respect to its center axis (1 a, 4 a, 7 a); applying layers (2 a-d; 5 a-d; 8 a-d ; 11) following in succession by means of an atomic layer deposition (ALD) method to faces (1 b-c; 4 b-c; 7 b-c) of the substrate (1, 4, 7) without rotation of the substrate (1, 4, 7) in order to form a coated substrate, and severing (3 a, b; 6 a, b; 9 a, b) at least one slice (13) from the coated substrate (1, 4, 7), by the coated substrate (1, 4, 7) being divided at least once at a right angle to the center axis (1 a, 4 a, 7 a).

Marcel Mayer

Papers

Multilayer Fresnel zone plate for soft X-ray microscopy resolves sub-39 nm structures

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

Multilayer Fresnel zone plates for high energy radiation resolve 21 nm features at 1.2 keV

Ion beam lithography for direct patterning of high accuracy large area X-ray elements in gold on membranes

Method and apparatus for producing a Fresnel zone plate