Corinne Grévent

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

Best resolutions in X-ray focusing are obtained to date by using diffractive lenses called Fresnel zone plates (FZPs). Their further improvement is nevertheless hindered by fundamental limitations in the employed manufacturing techniques. Here, we show a novel method to fabricate FZPs based on multilayer deposition with atomic layer deposition (ALD) and subsequent sectioning with focused ion beam (FIB). For the first time a multilayer FZP working in the soft X-ray range was prepared and could achieve the best resolution obtained so far for multilayer FZPs by resolving features below 39nm in size in a scanning soft X-ray microscope. The new technique presents high potential for high resolution microscopy in both the soft and hard X-ray range.

Rapid prototyping of Fresnel zone plates via direct Ga+ ion beam lithography for high-resolution x-ray imaging

A significant challenge to the wide utilization of X-ray microscopy lies in the difficulty in fabricating adequate high-resolution optics. To date, electron beam lithography has been the dominant technique for the fabrication of diffractive focusing optics called Fresnel zone plates (FZP), even though this preparation method is usually very complicated and is composed of many fabrication steps. In this work, we demonstrate an alternative method that allows the direct, simple, and fast fabrication of FZPs using focused Ga(+) beam lithography practically, in a single step. This method enabled us to prepare a high-resolution FZP in less than 13 min. The performance of the FZP was evaluated in a scanning transmission soft X-ray microscope where nanostructures as small as sub-29 nm in width were clearly resolved, with an ultimate cutoff resolution of 24.25 nm, demonstrating the highest first-order resolution for any FZP fabricated by the ion beam lithography technique. This rapid and simple fabrication scheme illustrates the capabilities and the potential of direct ion beam lithography (IBL) and is expected to increase the accessibility of high-resolution optics to a wider community of researchers working on soft X-ray and extreme ultraviolet microscopy using synchrotron radiation and advanced laboratory sources.

Ion beam lithography for Fresnel zone plates in X-ray microscopy

Fresnel Zone Plates (FZP) are to date very successful focusing optics for X-rays. Established methods of fabrication are rather complex and based on electron beam lithography (EBL). Here, we show that ion beam lithography (IBL) may advantageously simplify their preparation. A FZP operable from the extreme UV to the limit of the hard X-ray was prepared and tested from 450 eV to 1500 eV. The trapezoidal profile of the FZP favorably activates its 2nd order focus. The FZP with an outermost zone width of 100 nm allows the visualization of features down to 61, 31 and 21 nm in the 1st, 2nd and 3rd order focus respectively. Measured efficiencies in the 1st and 2nd order of diffraction reach the theoretical predictions.

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

The fabrication and performance of multilayer Al2O3/Ta2O5 Fresnel zone plates in the hard X-ray range and a discussion of possible future developments considering available materials are reported.

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

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.

Comparative study of ALD SiO2 thin films for optical applications

We have investigated the suitability of atomic layer deposition (ALD) for SiO2 optical coatings and applied it to broadband antireflective multilayers in combination with HfO2 as the high refractive index material. SiO2 thin films were successfully grown using tris[dimethylamino]silane (3DMAS), bis[diethylamino]silane (BDEAS) with plasma activated oxygen as precursors, and the AP-LTO330 precursor with ozone, respectively. The amorphous SiO2 films show very low optical losses within a spectral range of 200 nm to 1100 nm. Laser calorimetric measurements show absorption losses of 300 nm thick SiO2 films of about 1.5 parts per million at a wavelength of 1064 nm. The films are optically homogeneous and possess a good scalability of film thickness. The film surface porosity - which correlates to a shift in the transmittance spectra under vacuum and air conditions - has been suppressed by optimized plasma parameters or Al2O3 sealing layers.

High-resolution high-efficiency multilayer Fresnel zone plates for soft and hard x-rays

X-ray microscopy enables high spatial resolutions, high penetration depths and characterization of a broad range of materials. Calculations show that nanometer range resolution is achievable in the hard X-ray regime by using Fresnel zone plates (FZPs) if certain conditions are satisfied. However, this requires, among other things, aspect ratios of several thousands. The multilayer (ML) type FZPs, having virtually unlimited aspect ratios, are strong candidates to achieve single nanometer resolutions. Our research is focused on the fabrication of ML-FZPs which encompasses deposition of multilayers over a glass fiber via the atomic layer deposition (ALD), which is subsequently sliced in the optimum thickness for the X-ray energy by a focused ion beam (FIB). We recently achieved aberration free imaging by resolving 21 nm features with an efficiency of up to 12.5 %, the highest imaging resolution achieved by an ML-FZP. We also showed efficient focusing of 7.9 keV X-rays down to 30 nm focal spot size (FWHM). For resolutions below ~10 nm, efficiencies would decrease significantly due to wave coupling effects. To compensate this effect high efficiency, low stress materials have to be researched, as lower intrinsic stresses will allow fabrication of larger FZPs with higher number of zones, leading to high light intensity at the focus. As a first step we fabricated an ML-FZP with a diameter of 62 μm, an outermost zone width of 12 nm and 452 active zones. Further strategies for fabrication of high resolution high efficiency multilayer FZPs will also be discussed.

Recent advances in use of atomic layer deposition and focused ion beams for fabrication of Fresnel zone plates for hard x-rays

Developments and advances in the e-beam lithography (EBL) made it possible to reach resolutions in a single digit nanometer range in the soft x-ray microscopy using Fresnel Zone Plates (FZP). However, it is very difficult to fabricate efficient FZPs for hard x-rays via this conventional fabrication technique due to limitations in the achievable aspect ratios. Here, we demonstrate the use of alternative fabrication techniques that depend on utilization of atomic layer deposition and focused ion beam processing to deliver FZPs that are efficient for the hard X-ray range.

Overview of the multilayer-Fresnel zone plate and the kinoform lens development at MPI for Intelligent Systems

The ultimate goal of our research is to develop novel fabrication methods for high efficiency and high resolution X-ray optics. To this end, we have been pursuing the fabrication of several innovative diffractive/refractive optics designs. One such optic is the multilayer type Fresnel zone plate (ML-FZP). Our fabrication process relies on the atomic layer deposition (ALD) of two materials on a smooth glass fiber followed by a focused ion beam (FIB) based slicing and polishing. The ALD process allows much smaller outermost zone widths than the standard electron beam lithography based FZPs, meaning FZPs with potentially higher resolutions. Moreover, by depositing the multilayer on a cm long glass-fiber FZPs with very high optical thicknesses can be fabricated that can efficiently focus harder X-rays as well. A 21 nm half-pitch resolution was achieved using the ML-FZPs. Another optic we have been working on is the kinoform lens, which is a refractive/diffractive optic with a 100 % theoretical focusing efficiency. Their fabrication is usually realized by using approximate models which limit their success. Recently the fabrication of real kinoform lenses has been successfully realized in our lab via gray-scale direct-write ion beam lithography without any approximations. The lenses have been tested in the soft X-ray range achieving up to ~90 % of the calculated efficiency which indicates outstanding replication of the designed profile. Here we give an overview of our research and discuss the future challenges and opportunities for these optics.

Fabrication and X-ray testing of true kinoform lenses with high efficiencies

Kinoform lenses are focusing optics with a 100 % theoretical focusing efficiency. Up to date, the actual continuous 3D surface relief profiles of X-ray kinoform lenses could only be approximately fabricated. Now, we have come up with an effective ion beam lithography fabrication strategy producing first-ever imaging-quality circularly symmetric kinoform lenses which demonstrated reasonably high focusing efficiencies. Here, we will discuss the potential of the fabrication method and the utility of kinoform lenses enabled by it. Special emphases will be placed on materials development including selection and design, efficiency considerations for various energies and possible applications.