Gung-Chian Yin

30 nm resolution x-ray imaging at 8 keV using third order diffraction of a zone plate lens objective in a transmission microscope

A hard x-ray transmission microscope with 30nm spatial resolution has been developed employing the third diffraction order of a zone plate objective. The microscope utilizes a capillary type condenser with suitable surface figure to generate a hollow cone illumination which is matched in illumination range to the numerical aperture of the third order diffraction of a zone plate with an outmost zone width of 50nm. Using a test sample of a 150nm thick gold spoke pattern with finest half-pitch of 30nm, the authors obtained x-ray images with 30nm resolution at 8keV x-ray energy.

Energy-tunable transmission x-ray microscope for differential contrast imaging with near 60 nm resolution tomography

An energy-tunable transmission hard x-ray microscope with close to 60 nm spatial resolution in three dimensions (3D) has been developed. With a cone beam illumination, a zone plate of 50 nm outmost zone width, a stable mechanical design, and software feedback, we obtained tomographic data sets that are close to 60 nm spatial resolution. Meanwhile, the element specific imaging was also obtained by a differential absorption contrast technique used below and above the absorption of the element. Examples of advanced intergraded circuit devices are used to demonstrate the element selectivity and spatial resolution in 3D of the microscope.

X-ray beamlines for structural studies at the NSRRC superconducting wavelength shifter

Using a superconducting-wavelength-shifter X-ray source with a photon flux density of 10(11)-10(13) photons s(-1) mrad(-1) (0.1% bandwidth)(-1) (200 mA)(-1) in the energy range 5-35 keV, three hard X-ray beamlines, BL01A, BL01B and BL01C, have been designed and constructed at the 1.5 GeV storage ring of the National Synchrotron Radiation Research Center (NSRRC). These have been designed for structure-related research using X-ray imaging, absorption, scattering and diffraction. The branch beamline BL01A, which has an unmonochromatized beam, is suitable for phase-contrast X-ray imaging with a spatial resolution of 1 microm and an imaging efficiency of one frame per 10 ms. The main beamline BL01B has 1:1 beam focusing and a medium energy resolution of approximately 10(-3). It has been designed for small-angle X-ray scattering and transmission X-ray microscopy, used, respectively, in anomalous scattering and nanophase-contrast imaging with 30 nm spatial resolution. Finally, the branch beamline BL01C, which features collimating and focusing mirrors and a double-crystal monochromator for a high energy resolution of approximately 10(-4), has been designed for X-ray absorption spectroscopy and high-resolution powder X-ray diffraction. These instruments, providing complementary tools for studying multiphase structures, have opened up a new research trend of integrated structural study at the NSRRC, especially in biology and materials. Examples illustrating the performances of the beamlines and the instruments installed are presented.

Fabrication of high-aspect-ratio Fresnel zone plates by e-beam lithography and electroplating

The fabrication of gold Fresnel zone plates, by a combination of e-beam lithography and electrodeposition, with a 30 nm outermost zone width and a 450 nm-thick structure is described. The e-beam lithography process was implemented with a careful evaluation of applied dosage, tests of different bake-out temperatures and durations for the photoresist, and the use of a developer without methylisobutylketone. Electrodeposition with a pulsed current mode and with a specially designed apparatus produced the desired high-aspect-ratio nanostructures. The fabricated zone plates were examined by electron microscopy and their performances were assessed using a transmission X-ray microscope. The results specifically demonstrated an image resolution of 40 nm.

Imaging cells and sub-cellular structures with ultrahigh resolution full-field X-ray microscopy

Our experimental results demonstrate that full-field hard-X-ray microscopy is finally able to investigate the internal structure of cells in tissues. This result was made possible by three main factors: the use of a coherent (synchrotron) source of X-rays, the exploitation of contrast mechanisms based on the real part of the refractive index and the magnification provided by high-resolution Fresnel zone-plate objectives. We specifically obtained high-quality microradiographs of human and mouse cells with 29 nm Rayleigh spatial resolution and verified that tomographic reconstruction could be implemented with a final resolution level suitable for subcellular features. We also demonstrated that a phase retrieval method based on a wave propagation algorithm could yield good subcellular images starting from a series of defocused microradiographs. The concluding discussion compares cellular and subcellular hard-X-ray microradiology with other techniques and evaluates its potential impact on biomedical research.

Quantitative phase retrieval in transmission hard x-ray microscope

Quantitative phase retrieval with a sub-100-nm resolution is achieved from micrographs of a zone plate based transmission x-ray microscope. A plastic zone plate containing objects of sizes from micrometers down to tens of nanometers is used as a test sample to quantify the retrieved phase. Utilizing the focal serial images in the image plane, the phase information is retrieved quantitatively across the entire range of sizes by combining the transport intensity equation and self-consistent wave propagation methods in this partial coherence system. The study demonstrates a solution to overcome the deficiency encountered in the two phase retrieval approaches.

Hard X-ray Microscopy with sub 30 nm Spatial Resolution

A transmission X‐ray microscope (TXM) has been installed at the BL01B beamline at National Synchrotron Radiation Research Center in Taiwan. This state‐of‐the‐art TXM operational in a range 8‐11 keV provides 2D images and 3D tomography with spatial resolution 60 nm, and with the Zernike‐phase contrast mode for imaging light materials such as biological specimens. A spatial resolution of the TXM better than 30 nm, apparently the best result in hard X‐ray microscopy, has been achieved by employing the third diffraction order of the objective zone plate. The TXM has been applied in diverse research fields, including analysis of failure mechanisms in microelectronic devices, tomographic structures of naturally grown photonic specimens, and the internal structure of fault zone gouges from an earthquake core. Here we discuss the scope and prospects of the project, and the progress of the TXM in NSRRC.

Probing the exciton-phonon coupling strengths of O-polar and Zn-polar ZnO wafer using hard X-ray excited optical luminescence

The temperature-dependent hard X-ray excited optical luminescence (XEOL) spectroscopy was used to study the optical properties of O and Zn polarity of a c-plane single crystal ZnO wafer. By analyzing the XEOL and XRD, we found an unprecedented blue shift of the free exciton transition with increasing the excited carrier density as tuning the X-ray energy across the Zn K-edge, and the O-polar face possesses better crystal structure than the Zn-polar one. This spectral blue shift is attributed to the Coulomb screening of the spontaneous polarization by the excited free carriers that result in decreasing the exciton-phonon Frohlich interaction to reduce exciton binding energy.

X-ray nanoprobe project at Taiwan Photon Source

The hard X-ray nanoprobe facility at Taiwan Photon Source (TPS) provides versatile X-ray analysis techniques, with tens of nanometer resolution, including XRF, XAS, XEOL, projection microscope, CDI, etc. Resulting from the large numerical aperture obtained by utilizing Montel KB mirrors, the beamline with a moderate length 75 meters can conduct similar performance with those beamlines longer than 100 meters. The two silica-made Montel mirrors are 45 degree cut and placed in a V-shape to eliminate the gap loss and the deformation caused by gravity. The slope error of the KB mirror pair is less than 0.04 µrad accomplished by elastic emission machining (EEM) method. For the beamline, a horizontal DCM and two-stage focusing in horizontal direction is applied. For the endstation, a combination of SEM for quickly positioning the sample, a fly scanning system with laser interferometers, a precise temperature control system, and a load lock transfer system will be implemented. In this presentation, the design and...

Dark field image of full-field transmission hard X-ray microscope in 8-11 keV

We have demonstrated dark-field imaging using a full-field hard x-ray microscope by using a custom capillary-based condenser. The condenser provides illumination with a numeric aperture about 3-mrad with high efficiency. This high illumination angle allows full-resolution imaging using a 50 nm hard x-ray zone plate. The zeroth order beam from the condenser is well out of the zoneplate range - which allows a high signal-to-noise ratio in the image plane. Small particles with high scattering power, such as colloidal gold markers used in biology are well-suited for dark-field imaging. Combining with high brightness source from NSRRC BL01B, the dark field image can be acquired within several minutes with high contrast ratio. In this paper, the dark field image of IC and the zoneplate defect will be demonstrated and studied in different energy under dark field mode.