Pascal Meyer

DoseSim: Microsoft-Windows graphical user interface for using synchrotron x-ray exposure and subsequent development in the LIGA process

The LIGA process, which combines x-ray lithography with electroplating and moulding, is a technique used worldwide for the fabrication of high aspect ratio microstructures. In the first step (x-ray lithography), a resist layer is applied to a metal-coated substrate, which is then patterned by shadow printing through an x-ray mask with synchrotron radiation. The second step consists in dissolving the exposed parts or the unexposed parts, of a positive and negative resist, respectively, in an organic developer. A graphical user interface has been developed, working under Windows, which meets the necessary requirements of a LIGA x-ray beamline. The code currently permits the computation of synchrotron radiation from bending magnets, the effects of the optical properties of materials, and the necessary parameters for the resist exposure. Also, this program is highly flexible and allows the user to access many annexed calculation possibilities, for example, optimization of the absorber thickness for a desired dose after the absorber, filter possibilities for a desired ratio top dose/bottom dose, calculation of the necessary time to develop the exposed resist. The comparison of results of this code and data used by different x-ray LIGA centers will be given. A general overview of the possibilities of this program will be presented.

Quantitative imaging using high-energy X-ray phase-contrast CT with a 70 kVp polychromatic X-ray spectrum

Imaging of large and dense objects with grating-based X-ray phase-contrast computed tomography requires high X-ray photon energy and large fields of view. It has become increasingly possible due to the improvements in the grating manufacturing processes. Using a high-energy X-ray phase-contrast CT setup with a large (10 cm in diameter) analyzer grating and operated at an acceleration tube voltage of 70 kVp, we investigate the complementarity of both attenuation and phase contrast modalities with materials of various atomic numbers (Z). We confirm experimentally that for low-Z materials, phase contrast yields no additional information content over attenuation images, yet it provides increased contrast-to-noise ratios (CNRs). The complementarity of both signals can be seen again with increasing Z of the materials and a more comprehensive material characterization is thus possible. Imaging of a part of a human cervical spine with intervertebral discs surrounded by bones and various soft tissue types showcases the benefit of high-energy X-ray phase-contrast system. Phase-contrast reconstruction reveals the internal structure of the discs and makes the boundary between the disc annulus and nucleus pulposus visible. Despite the fact that it still remains challenging to develop a high-energy grating interferometer with a broad polychromatic source with satisfactory optical performance, improved image quality for phase contrast as compared to attenuation contrast can be obtained and new exciting applications foreseen.

In-vivo X-ray Dark-Field Chest Radiography of a Pig

X-ray chest radiography is an inexpensive and broadly available tool for initial assessment of the lung in clinical routine, but typically lacks diagnostic sensitivity for detection of pulmonary diseases in their early stages. Recent X-ray dark-field (XDF) imaging studies on mice have shown significant improvements in imaging-based lung diagnostics. Especially in the case of early diagnosis of chronic obstructive pulmonary disease (COPD), XDF imaging clearly outperforms conventional radiography. However, a translation of this technique towards the investigation of larger mammals and finally humans has not yet been achieved. In this letter, we present the first in-vivo XDF full-field chest radiographs (32 × 35 cm2) of a living pig, acquired with clinically compatible parameters (40 s scan time, approx. 80 µSv dose). For imaging, we developed a novel high-energy XDF system that overcomes the limitations of currently established setups. Our XDF radiographs yield sufficiently high image quality to enable radiographic evaluation of the lungs. We consider this a milestone in the bench-to-bedside translation of XDF imaging and expect XDF imaging to become an invaluable tool in clinical practice, both as a general chest X-ray modality and as a dedicated tool for high-risk patients affected by smoking, industrial work and indoor cooking.

Large field-of-view tiled grating structures for X-ray phase-contrast imaging

X-ray grating-based interferometry promises unique new diagnostic possibilities in medical imaging and materials analysis. To transfer this method from scientific laboratories or small-animal applications to clinical radiography applications, compact setups with a large field of view (FoV) are required. Currently the FoV is limited by the grating area, which is restricted due to the complex manufacturing process. One possibility to increase the FoV is tiling individual grating tiles to create one large area grating mounted on a carrier substrate. We investigate theoretically the accuracy needed for a tiling process in all degrees of freedom by applying a simulation approach. We show how the resulting precision requirements can be met using a custom-built frame for exact positioning. Precise alignment is achieved by comparing the fringe patterns of two neighboring grating tiles in a grating interferometer. With this method, the FoV can be extended to practically any desired length in one dimension. First results of a phase-contrast scanning setup with a full FoV of 384 mm × 24 mm show the suitability of this method.

Time resolved X-ray Dark-Field Tomography Revealing Water Transport in a Fresh Cement Sample

Grating-based X-ray dark-field tomography is a promising technique for biomedical and materials research. Even if the resolution of conventional X-ray tomography does not suffice to resolve relevant structures, the dark-field signal provides valuable information about the sub-pixel microstructural properties of the sample. Here, we report on the potential of X-ray dark-field imaging to be used for time-resolved three-dimensional studies. By repeating consecutive tomography scans on a fresh cement sample, we were able to study the hardening dynamics of the cement paste in three dimensions over time. The hardening of the cement was accompanied by a strong decrease in the dark-field signal pointing to microstructural changes within the cement paste. Furthermore our results hint at the transport of water from certain limestone grains, which were embedded in the sample, to the cement paste during the process of hardening. This is indicated by an increasing scattering signal which was observed for two of the six tested limestone grains. Electron microscopy images revealed a distinct porous structure only for those two grains which supports the following interpretation of our results. When the water filled pores of the limestone grains empty during the experiment the scattering signal of the grains increases.

X-ray grating interferometry at photon energies over 180 keV

We report on the implementation and characterization of grating interferometry operating at an x-ray energy of 183 keV. With the possibility to use this technique at high x-ray energies, bigger specimens could be studied in a quantitative way. Also, imaging strongly absorbing specimens will benefit from the advantages of the phase and dark-field signals provided by grating interferometry. However, especially at these high photon energies the performance of the absorption grating becomes a key point on the quality of the system, because the grating lines need to keep their small width of a couple of micrometers and exhibit a greater height of hundreds of micrometers. The performance of high aspect ratio absorption gratings fabricated with different techniques is discussed. Further, a dark-field image of an alkaline multicell battery highlights the potential of high energy x-ray grating based imaging.

Development behavior of irradiated foils and microstructures

The LIGA process, which combines x-ray lithography with electroplating and modeling, is a world wide used technique for the fabrication of high aspect ratio microstructures. In the first step a resist layer, typically PMMA, which is applied to a metal coated substrate, is patterned by shadow printing through a x-ray mask with synchrotron radiation. The exposed parts are subsequently dissolved in an organic developer. The achievable quality of the microstructure is decisively defined by the development process. In order to define an effective development process and create a simulation tool, which allows to foretell the needed development parameters and the achievable quality already at a design stage, the development behavior and its influencing parameters need to be investigated. Much work has been done in this area. In these previous studies, the development rate was either studied using PMMA foils in which a homogeneous dose or a dose profile has been deposited, or using irradiated microstructures. In the first case, result obtained by ex-situ measurements show, that the development rate is a bare function of the dose. In case of irradiated microstructures, the experimentally obtained development rate was described as an empirical function of the dose value and depth of dose deposition. The aim of this work is to investigate the difference in the development behavior of a microstructure compared to a foil and to link the results. Therefore, using in-situ measurements, we have made experiments using foils and microstructures with crosslinked and non-crosslinked PMMA covering a wide dose range. The final purpose is to find a relation between dose and development rate to determine the necessary development time of a sample with a given dose profile, with high precision. Experiments, result and simulation of the development rate, for the two kinds of materials are presented and discussed.

On the origin and nature of the grating interferometric dark-field contrast obtained with low-brilliance x-ray sources.

The x-ray dark-field contrast accessible via grating interferometry is sensitive to features at length scales well below what is resolvable by a detector system. It is commonly explained as arising from small-angle x-ray scattering (SAXS), and can be implemented both at synchrotron beamlines and with low-brilliance sources such as x-ray tubes. Here, we demonstrate that for tube based setups the underlying process of image formation can be fundamentally different. For focal spots or detector pixels that comprise multiple grating periods, we show that dark-field images contain a strong artificial and system-specific component not arising from SAXS. Based on experiments carried out with a nanofocus x-ray tube and the example of an excised rat lung, we demonstrate that the dark-field contrast observed for porous media transforms into a differential phase contrast for large geometric magnifications. Using a photon counting detector with an adjustable point spread function, we confirm that a dark-field image can indeed be formed by an intra-pixel differential phase contrast that cannot be resolved as such due to a dephasing between the periodicities of the absorption grating and the Talbot carpet. Our findings are further corroborated by a link between the strength of this pseudo-dark-field contrast and our x-ray tubes focal spot size in a three-grating setup. These results must not be ignored when measurements are intended to be reproducible across systems.

Note: Gratings on low absorbing substrates for x-ray phase contrast imaging

Grating based X-ray phase contrast imaging is on the verge of being applied in clinical settings. To achieve this goal, compact setups with high sensitivity and dose efficiency are necessary. Both can be increased by eliminating unwanted absorption in the beam path, which is mainly due to the grating substrates. Fabrication of gratings via deep X-ray lithography can address this issue by replacing the commonly used silicon substrate with materials with lower X-ray absorption that fulfill certain boundary conditions. Gratings were produced on both graphite and polymer substrates without compromising on structure quality. These gratings were tested in a three-grating setup with a source operated at 40 kVp and lead to an increase in the detector photon count rate of almost a factor of 4 compared to a set of gratings on silicon substrates. As the visibility was hardly affected, this corresponds to a significant increase in sensitivity and therefore dose efficiency.

Increasing the aperture of x-ray mosaic lenses by freeze drying

Point focus x-ray mosaic lenses are limited in aperture by the aspect ratio that can be reached in the micro fabrication process. In lithography based micro fabrication processes, which are used to fabricate the lens pillar structures, the achievable aspect ratio is restricted by structure collapse due to capillary forces which occur during drying after development. Capillary forces can be avoided by freeze drying, hence avoiding the direct phase change from liquid to gas. Substituting conventional drying by freeze drying using cyclohexane at a temperature of  −10 °C, we could increase the achievable aspect ratio for the triangular pillar structures with edge length of 10 to 45 µm of the x-ray mosaic lenses by up to a factor of 2.2 with no further changes in process, material or structural geometry. A maximum aspect ratio of 30 was achieved for pillars with 10 µm edge length. The process can readily be employed to other structures or lithography techniques.