Andrei Tkachuk

X-ray computed tomography in Zernike phase contrast mode at 8 keV with 50-nm resolution using Cu rotating anode X-ray source

High-resolution X-ray computed tomography (XCT) enables nondestructive 3D imaging of complex structures, regardless of their state of crystallinity. This work describes a sub-50 nm resolution XCT system operating at 8 keV in absorption and Zernike phase contrast modes based on a commercially available Cu rotating anode laboratory X-ray source. The system utilizes a high efficiency reflective capillary condenser lens and high-resolution Fresnel zone plates with an outermost zone width of 35 nm and 700 nm structure height resulting in a spatial resolution better than 50 nm currently. Imaging a fragment of the solid oxide fuel cells (SOFC) with 50 nm resolution is presented as an application example of the XCT technique in materials science and nanotechnology.

Automated markerless full field hard x-ray microscopic tomography at sub-50 nm 3-dimension spatial resolution

A full field transmission x-ray microscope (TXM) has been developed and commissioned at the National Synchrotron Light Source at Brookhaven National Laboratory. The capabilities we developed in auto-tomography, local tomography, and spectroscopic imaging that overcome many of the limitations and difficulties in existing transmission x-ray microscopes are described and experimentally demonstrated. Sub-50 nm resolution in 3-dimension (3D) with markerless automated tomography has been achieved. These capabilities open up scientific opportunities in many research fields.

Nanoscale X-Ray Microscopic Imaging of Mammalian Mineralized Tissue

A novel hard transmission X-ray microscope (TXM) at the Stanford Synchrotron Radiation Lightsource operating from 5 to 15 keV X-ray energy with 14 to 30 microm2 field of view has been used for high-resolution (30-40 nm) imaging and density quantification of mineralized tissue. TXM is uniquely suited for imaging of internal cellular structures and networks in mammalian mineralized tissues using relatively thick (50 microm), untreated samples that preserve tissue micro- and nanostructure. To test this method we performed Zernike phase contrast and absorption contrast imaging of mouse cancellous bone prepared under different conditions of in vivo loading, fixation, and contrast agents. In addition, the three-dimensional structure was examined using tomography. Individual osteocytic lacunae were observed embedded within trabeculae in cancellous bone. Extensive canalicular networks were evident and included processes with diameters near the 30-40 nm instrument resolution that have not been reported previously. Trabecular density was quantified relative to rod-like crystalline apatite, and rod-like trabecular struts were found to have 51-54% of pure crystal density and plate-like areas had 44-53% of crystal density. The nanometer resolution of TXM enables future studies for visualization and quantification of ultrastructural changes in bone tissue resulting from osteoporosis, dental disease, and other pathologies.

Ellipsoidal and parabolic glass capillaries as condensers for x-ray microscopes

Single-bounce ellipsoidal and paraboloidal glass capillary focusing optics have been fabricated for use as condenser lenses for both synchrotron and tabletop x-ray microscopes in the x-ray energy range of 2.5-18 keV. The condenser numerical apertures (NAs) of these devices are designed to match the NA of x-ray zone plate objectives, which gives them a great advantage over zone plate condensers in laboratory microscopes. The fabricated condensers have slope errors as low as 20 murad rms. These capillaries provide a uniform hollow-cone illumination with almost full focusing efficiency, which is much higher than what is available with zone plate condensers. Sub-50 nm resolution at 8 keV x-ray energy was achieved by utilizing this high-efficiency condenser in a laboratory microscope based on a rotating anode generator.

A 30 nm-resolution hard X-ray microscope with X-ray fluorescence mapping capability at BSRF

A full-field transmission X-ray microscope (TXM) operating continuously from 5 keV to 12 keV with fluorescence mapping capability has been designed and constructed at the Beijing Synchrotron Radiation Facility, a first-generation synchrotron radiation facility operating at 2.5 GeV. Spatial resolution better than 30 nm has been demonstrated using a Siemens star pattern in both absorption mode and Zernike phase-contrast mode. A scanning-probe mode fluorescence mapping capability integrated with the TXM has been shown to provide 50 p.p.m. sensitivity for trace elements with a spatial resolution (limited by probing beam spot size) of 20 µm. The optics design, testing of spatial resolution and fluorescence sensitivity are presented here, including performance measurement results.

MISTRAL: a transmission soft X-ray microscopy beamline for cryo nano-tomography of biological samples and magnetic domains imaging.

The performance of MISTRAL is reported, the soft X-ray transmission microscopy beamline at the ALBA light source (Barcelona, Spain) which is primarily dedicated to cryo soft X-ray tomography (cryo-SXT) for three-dimensional visualization of whole unstained cells at spatial resolutions down to 30 nm (half pitch). Short acquisition times allowing for high-throughput and correlative microscopy studies have promoted cryo-SXT as an emerging cellular imaging tool for structural cell biologists bridging the gap between optical and electron microscopy. In addition, the beamline offers the possibility of imaging magnetic domains in thin magnetic films that are illustrated here with an example.

A high resolution, hard x-ray bio-imaging facility at SSRL

The old saying that seeing is believing has particular resonance for studying biological cells and tissues. Since 1677, when Anton van Leeuwenhoek used a simple light microscope to discover single cell organisms, scientists have relied on structural information obtained from microscopes with improving capabilities to advance the understanding of how biological systems work. Optical and electron microscopes are essential for many of these important discoveries and have been widely employed in biomedical research laboratories. However, various limitations exist in these microscopy techniques. We describe below how the new X-ray imaging facility at the Stanford Synchrotron Radiation Laboratory (SSRL), based on an Xradia nano-XCT full-field transmission X-ray microscope (TXM), can provide complementary and unique capabilities to the current microscopy methods for studying complex biological systems.

In Situ Surface X-Ray Scattering Observation of Long-Range Ordered ( 19 × 19 ) R23.4 ° ­ 13 CO Structure on Pt(111) in Aqueous Electrolytes

Presented herein is the experimental observation of the long-range ordered (√19 × √19)R23.4°-13CO structure on Pt(111) in aqueous electrolytes by in situ surface X-ray scattering. The results confirmed the presence of two mirrored domains suggested earlier on the basis of scanning tunneling microscopy and infrared measurements. Based on the weak intensity of the second order adlattice reflections and earlier results obtained by other techniques, a further refinement of the (√19 × √19) structure with tilted CO molecules is proposed. The hystereses observed in transitions between (2 × 2 )- 3 CO and (√19 × √19)R23.4°-13CO phases, as well as in CO adsorption and stripping, with change in electrode potential are discussed.

High-resolution x-ray tomography using laboratory sources

X-ray computed tomography (XCT) is a powerful nondestructive 3D imaging technique, which enables the visualization of the three dimensional structure of complex, optically opaque samples. High resolution XCT using Fresnel zone plate lenses has been confined in the past to synchrotron radiation centers due to the need for a bright and intense source of x-rays. This confinement severely limits the availability and accessibility of x-ray microscopes and the wide proliferation of this methodology. We are describing a sub-50nm resolution XCT system operating at 8 keV in absorption and Zernike phase contrast mode based on a commercially available laboratory x-ray source. The system utilizes high-efficiency Fresnel zone plates with an outermost zone width of 35 nm and 700 nm structure height resulting in a current spatial resolution better than 50 nm. In addition to the technical description of the system and specifications, we present application examples in the semiconductor field.

Non invasive, multiscale 3D X-Ray characterization of porous functional composites and membranes, with resolution from MM to sub 50 NM

We describe a novel x-ray computer tomography (CT) system for high contrast, non invasive 3D imaging of internal structures of functional ceramics, composites and polymeric membranes. System is capable of multi-length scale imaging from mm to sub 50 nm spatial resolutions and requires little or no sample preparation or staining. Relatively large samples with thickness from several mm to several microns may be imaged at high resolution. Examples using functional composites and membranes from SOFC (solid oxide fuel cell) and PEM (proton exchange membranes) fuel cell to derive direct information such as porosity and catalytic membrane degradation will be discussed. The key to the novel laboratory CT technology lies in utilizing proprietary x-ray optics with Fresnel Zone plates, and innovative high resolution, high contrast detectors.