Heinrich Riesemeier

Investigation of water evolution and transport in fuel cells with high resolution synchrotron x-ray radiography

The authors report on in situ investigations of liquid water evolution and transport in an undisturbed operating fuel cell at the microscopic level. Synchrotron x-ray radiography enhances the spatial resolution by two orders of magnitude compared to the state-of-the-art techniques in this field. The primary spots of liquid water formation, their growth, and transport inside the porous gas diffusion material were analyzed; correlations between operating conditions and the dynamics of droplet formation are described. Previous findings from modeling and simulation approaches are confirmed and the applicability for the description of in situ processes of a recently proposed model has been proven.

A new experimental station for simultaneous X-ray microbeam scanning for small- and wide-angle scattering and fluorescence at BESSY II

A new instrument for simultaneous microbeam small- and wide-angle X-ray scattering and X-ray fluorescence (SAXS/WAXS/XRF) is presented. The instrument is installed at the microfocus beamline at BESSY II and provides a beam of 10 µm size with a flux of about 109 photons s−1. A SAXS resolution up to 500 A d-spacing and a range of scattering vectors of almost three orders of magnitude are reached by using a large-area high-resolution CCD-based detector for simultaneous SAXS/WAXS. The instrument is particularly suited for scanning SAXS/WAXS/XRF experiments on hierarchically structured biological tissues. The necessary infrastructure, such as a cryo-stream facility and an on-site preparation laboratory for biological specimens, are available.

Detection system for microimaging with neutrons

A new high-resolution detector setup for neutron imaging has been developed based on infinity-corrected optics with high light collection, combined with customized mounting hard- ware. The system can easily be installed, handled and fitted to any existing facility, avoiding the necessity of complex optical systems or further improved electronics (CCD). This is the first time optical magnification higher than 1:1 has been used with scintillator-based neutron detectors, as well as the first implementation of infinity corrected optics for neutron imaging, achieving the smallest yet reported effective pixel size of 3.375 mm. A novel transparent crystal scintillator (GGG crystal) has been implemented with neutrons for the first time to overcome limitations of traditional powder scintillators (Li6/ZnS, Gadox). The standardized procedure for resolution mea- surements with the Modulation Transfer Function (MTF) is summarized to facilitate comparison between instruments and facilities. Using this new detector setup, a resolution of 14.8 mm with a field of view of 6 mm�6 mm has been achieved while maintaining reasonable count times. These advances open a wide range of new possible research applications and allow the potential for additional future developments.

In situ investigation of the discharge of alkaline Zn–MnO2 batteries with synchrotron x-ray and neutron tomographies

Zn–MnO2 alkaline batteries were investigated in situ at different stages of electric discharge by synchrotron tomography with monochromatic x rays and by neutron tomography. The spatial distribution and the changes in the morphology of different components of a battery caused by the reduction of MnO2, the dissolution of Zn, and the nucleation and growth of ZnO are investigated with high spatial resolution around several micrometers with x rays. Neutron tomography is used to monitor the changes in the spatial distribution of hydrogen in the MnO2 matrix and provides complementary information about the process.

Going beyond histology. Synchrotron micro-computed tomography as a methodology for biological tissue characterization: from tissue morphology to individual cells

Current light microscopic methods such as serial sectioning, confocal microscopy or multiphoton microscopy are severely limited in their ability to analyse rather opaque biological structures in three dimensions, while electron optical methods offer either a good three-dimensional topographic visualization (scanning electron microscopy) or high-resolution imaging of very thin samples (transmission electron microscopy). However, sample preparation commonly results in a significant alteration and the destruction of the three-dimensional integrity of the specimen. Depending on the selected photon energy, the interaction between X-rays and biological matter provides semi-transparency of the specimen, allowing penetration of even large specimens. Based on the projection-slice theorem, angular projections can be used for tomographic imaging. This method is well developed in medical and materials science for structure sizes down to several micrometres and is considered as being non-destructive. Achieving a spatial and structural resolution that is sufficient for the imaging of cells inside biological tissues is difficult due to several experimental conditions. A major problem that cannot be resolved with conventional X-ray sources are the low differences in density and absorption contrast of cells and the surrounding tissue. Therefore, X-ray monochromatization coupled with a sufficiently high photon flux and coherent beam properties are key requirements and currently only possible with synchrotron-produced X-rays. In this study, we report on the three-dimensional morphological characterization of articular cartilage using synchrotron-generated X-rays demonstrating the spatial distribution of single cells inside the tissue and their quantification, while comparing our findings to conventional histological techniques.

In vitro synchrotron-based radiography of micro-gap formation at the implant–abutment interface of two-piece dental implants

Micro-radiography using hard X-ray synchrotron radiation is the first potential tool to allow an evaluation of the mechanical behavior of the dental implant–abutment complex during force application, thus enabling the enhancement of the design of dental implants which has been based on theoretical analysis to date.

RBS, SY-XRF, INAA and ICP-IDMS of Antimony Implanted in Silicon. A Multi-Method Approach to Characterize and Certify a Reference Material.

A layer of Sb atoms, implanted with an energy of 400 keV and a nominal dose of 5×1016 atoms/cm2 into a high purity silicon wafer, was certified for its areal density (atoms/cm2) using Rutherford backscattering spectrometry (RBS), instrumental neutron activation analysis (INAA) and inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) and for its isotope ratio using INAA and ICP-IDMS. Excellent agreement between the results of the different independent methods was found. In the present work, the measurements of the homogeneity of the areal density of Sb, previously determined with RBS in spots having 1 mm diameter, are improved with synchrotron X-ray fluorescence analysis: Higher precision in even smaller sample spots allows to estimate a reduced inhomogeneity of the whole batch of samples of the order of only 0.4%. Thus the uncertainty of the certified value can further be reduced. Down to fractions of a chip with 0.3×0.4 mm2 area, the areal density is now certified as (4.81±0.06)×1016 Sb atoms/cm2, where the expanded uncertainty 0.06 (coverage factor k=2) corresponds to only 1.2%. The relative merits of the different analytical methods are discussed.

Fresnel-propagated imaging for the study of human tooth dentin by partially coherent x-ray tomography

Recent methods of phase imaging in x-ray tomography allow the visualization of features that are not resolved in conventional absorption microtomography. Of these, the relatively simple setup needed to produce Fresnel-propagated tomograms appears to be well suited to probe tooth-dentin where composition as well as microstructure vary in a graded manner. By adapting analytical propagation approximations we provide predictions of the form of the interference patterns in the 3D images, which we compare to numerical simulations as well as data obtained from measurements of water immersed samples. Our observations reveal details of the tubular structure of dentin, and may be evaluated similarly to conventional absorption tomograms. We believe this exemplifies the power of Fresnel-propagated imaging as a form of 3D microscopy, well suited to quantify gradual microstructural-variations in teeth and similar tissues.

An in vitro pilot study of abutment stability during loading in new and fatigue-loaded conical dental implants using synchrotron-based radiography.

PURPOSE The implant-abutment connection of a two-piece dental implant exhibits complex micromechanical behavior. A microgap is evident at the implant-abutment interface, even in the virgin state, and its width varies when an external mechanical load is applied. MATERIALS AND METHODS This study used high-resolution synchrotron-based radiography in combination with hard x-ray phase-contrast mode to visualize this gap and estimate its size. Commercially available implants with different internal conical implant-abutment connections were imaged. Pairs of implants were imaged as manufactured (new) and after fatigue loading (5 million cycles up to 120 N). Then, different static loads were applied at different angles relative to the implant-abutment assemblies, and the implant-abutment microgaps were measured and compared. RESULTS Microgaps existed in all systems. Fatigue loading extended the size of the microgap and increased the possibility of micromovement of the implant-abutment complex. The cone angle of the connection also influenced the stability of the abutment, with flatter cones appearing to be more stable. CONCLUSION Cyclic loading at medium force (120 N) induces plastic deformation of titanium implants and abutments.

Imaging of articular cartilage – Data matching using X-ray tomography, SEM, FIB slicing and conventional histology

The study was aimed at demonstrating a true cellular resolution for articular cartilage using synchrotron radiation-based X-ray microcomputed tomography (SR-μCT) with a sample-specific optimization of the phase contrast. The generated tomographic data were later used to prepare a matching histological sample from the full volume specimen. We used highly coherent and monochromatic X-rays from a synchrotron source to image a tissue sample of bovine articular cartilage after deparaffinization. Phase contrast enhancement was achieved by using five different sample to detector distances for the same X-ray energy. After tomography, the sample was re-embedded into resin while retaining a dedicated sample orientation for subsequent sectioning and polishing, which was conducted until a previously defined spatial position was achieved. The protocol for resin embedding was developed to inhibit morphological changes during embedding. Giemsa staining was applied for better structural and morphological discrimination. Data from tomography and lightmicroscopy were exactly matched and finally compared to results from FIB/SEM imaging. Image detail was achieved at a single cell resolution. Image detail was achieved at a single cell resolution, which has been estimated to be 0.833μm/voxel in the tomographic data. SR-μCT with optimized phase contrast properties represents a method to investigate biological tissues in certain areas of interest, where true cellular resolution or enhanced volumetric imaging is needed. In this study, we demonstrate that this method can compete with conventional histology using light microscopy but even surpasses it due to the possibility of retrieving volumetric data.