Quantum Dot‐Based Thermal Spectroscopy and Imaging of Optically Trapped Microspheres and Single Cells

Laser‐induced thermal effects in optically trapped microspheres and single cells are investigated by quantum dot luminescence thermometry. Thermal spectroscopy has revealed a non‐localized temperature distribution around the trap that extends over tens of micrometers, in agreement with previous theoretical models besides identifying water absorption as the most important heating source. The experimental results of thermal loading at a variety of wavelengths reveal that an optimum trapping wavelength exists for biological applications close to 820 nm. This is corroborated by a simultaneous analysis of the spectral dependence of cellular heating and damage in human lymphocytes during optical trapping. This quantum dot luminescence thermometry demonstrates that optical trapping with 820 nm laser radiation produces minimum intracellular heating, well below the cytotoxic level (43 °C), thus, avoiding cell damage.     

A synchrotron radiation X-ray topographic study of the beam stability and perfection of some organic single crystals

An assessment is presented of the stability of some organic single crystals on exposure to an intense source of synchrotron radiation during X-ray topography examination. Examples are shown of the variations in defect structure of organic crystals prepared by different growth techniques. This study defines the applicability of a synchrotron radiation source for topographic examination of organic materials.     

ELECTROFORMING TECHNIQUES IN THE LIGA PROCESS FOR THE PRODUCTION OF MICRODEVICES

At the Karlsruhe Nuclear Research Center a new technology, called LIGA process, is being developed. In this process, synchrotron radiation lithography, electroforming and plastic molding are employed for the fabrication of microdevices with characteristic dimensions of few micrometers and structural heights of several hundred micrometers. Besides the production of metallic microdevices made of nickel, copper or gold, electroforming techniques are also used in fabricating X-ray masks and mold inserts to be utilized in the process. Plating processes used In the LIGA process are being automated for integration in a new clean-room plating machine developed for the mass production of microdevices.     

Applications of short-coherence digital holography in microscopy

We present an optical system based on short-coherence digital holography suitable for the imaging of three-dimensional microscopic objects. The short temporal coherence properties of the light source allow optical sectioning of the sample. Proper reconstruction of different layers within biological samples is possible up to a depth of a few hundred micrometers, but multiple scattering and inhomogeneities in the refractive index reduce the imaging quality for deeper layers. We have studied the possibility of numerically correcting sample-induced aberrations, and we now propose a method of improving image quality. Numerical simulations and preliminary experimental results show that compensation of these aberrations is possible to some extent.     

In-situ optical reflectance and synchrotron X-ray topography study of defects in epitaxial dilute GaAsN on GaAs

In order to investigate the possibilities of in-situ monitoring of GaAsN bulk layer growth and the crystal quality concerning the formation of misfit dislocations, GaAsN bulk samples with different layer thicknesses were grown using a metal-organic vapor phase epitaxy system equipped with a normal incidence optical reflectance setup. High-resolution X-ray diffractometry and synchrotron radiation X-ray topography were used to characterize the samples after growth. Combining the results from topography images and in-situ reflectance data, the formation of the misfit dislocations can be roughly identified from the reflectance curves and thus observed during growth.     

同步辐射原位X射线散射技术在纳米与能源材料中的应用

同步辐射原位X射线散射技术可以实现对材料结构进行多尺度的、无损的、高时间空间分辨率的表征,动态地揭示材料微观结构在不同外界环境下的演变过程。X射线散射基础理论已经相对成熟。第三代同步辐射光源大幅提高了X射线散射技术的时空分辨率,进一步拓宽X射线散射技术的应用场景。当前同步辐射原位X射线散射技术的难点主要集中于实验装置设计和大数据处理。概述了X射线散射技术的主要分类和基本的实验方法,主要介绍了不同分类的同步辐射原位X射线散射技术在纳米材料(纳米颗粒生长和纳米颗粒自组装)与能源材料(以钙钛矿薄膜材料为代表)研究中的应用。最后结合当前国内外先进同步辐射光源的发展现状,展望了同步辐射原位X射线散射技术未来发展的方向和应用前景。     

Controlling DNA capture and propagation through artificial nanopores

Electrophorescing biopolymers across nanopores modulates the ionic current through the pore, revealing the polymer's diameter, length, and conformation. The rapidity of polymer translocation ( approximately 30,000 bp/ms) in this geometry greatly limits the information that can be obtained for each base. Here we show that the translocation speed of lambda-DNA through artificial nanopores can be reduced using optical tweezers. DNAs coupled to optically trapped beads were presented to nanopores. DNAs initially placed up to several micrometers from the pore could be captured. Subsequently, the optical tweezers reduced translocation speeds to 150 bp/ms, about 200-fold slower than free DNA. Moreover, the optical tweezers allowed us to "floss" single polymers back and forth through the pore. The combination of controlled sample presentation, greatly slowed translocation speeds, and repeated electrophoresis of single DNAs removes several barriers to using artificial nanopores for sequencing, haplotyping, and characterization of protein-DNA interactions.     

A microdiffraction set-up for nanoporous metal-organic-framework-type solids

For the past decade, the emerging class of porous metal-organic frameworks has been becoming one of the most promising materials for the construction of extralarge pore networks in view of potential applications in catalysis, separation and gas storage. The knowledge of the atomic arrangements in these crystalline compounds is a key point for the understanding of the chemical and physical properties. Their crystal size limits the use of single-crystal diffraction analysis, and synchrotron radiation facilities may allow for the analysis of tiny crystals. We present here a microdiffraction set-up for the collection of Bragg intensities, which pushes down the limit to the micrometre scale by using a microfocused X-ray beam of 1 mum. We report the structure determination of a new porous metal-organic-framework-type aluminium trimesate (MIL-110) from a single crystal of a few micrometres length, showing very weak scattering factors owing to the composition of the framework (light elements) and very low density. Its structure is built up from a honeycomb-like network with hexagonal 16 A channels, involving the connection of octahedrally coordinated aluminium octameric motifs with the trimesate ligands. Solid-state NMR (27Al,13C,1H) and molecular modelling are finally considered for the structural characterization.     

同步辐射与分析测试

本文介绍一种大科学装置——同步辐射装置。这是一种数百人可同时在其上进行不同的科学技术实验的设备，其可达到的水平比实验室的极限水平高许多，从某些角度代表了国家的科学和技术水平。本文扼要介绍了同步辐射的特性，同步辐射装置的构造及一些主要的分析测试技术，如：X射线吸收精细结构光谱，X射线散射，高分辨X射线衍射，能量色散与时间分辨技术，聚集与微分析，成像与显微放大，综合测试原位测试及作铯对标定等。     

Laser Heating Tunability by Off‐Resonant Irradiation of Gold Nanoparticles

Temperature changes in the vicinity of a single absorptive nanostructure caused by local heating have strong implications in technologies such as integrated electronics or biomedicine. Herein, the temperature changes in the vicinity of a single optically trapped spherical Au nanoparticle encapsulated in a thermo‐responsive poly(N‐isopropylacrylamide) shell (Au@pNIPAM) are studied in detail. Individual beads are trapped in a counter‐propagating optical tweezers setup at various laser powers, which allows the overall particle size to be tuned through the phase transition of the thermo‐responsive shell. The experimentally obtained sizes measured at different irradiation powers are compared with average size values obtained by dynamic light scattering (DLS) from an ensemble of beads at different temperatures. The size range and the tendency to shrink upon increasing the laser power in the optical trap or by increasing the temperature for DLS agree with reasonable accuracy for both approaches. Discrepancies are evaluated by means of simple models accounting for variations in the thermal conductivity of the polymer, the viscosity of the aqueous solution and the absorption cross section of the coated Au nanoparticle. These results show that these parameters must be taken into account when considering local laser heating experiments in aqueous solution at the nanoscale. Analysis of the stability of the Au@pNIPAM particles in the trap is also theoretically carried out for different particle sizes.     

Spatially resolved analysis of small particles by confocal Raman microscopy: depth profiling and optical trapping

Raman microscopy is a powerful method to provide spatially resolved information about the chemical composition of materials. With confocal collection optics, the method is well suited to the analysis of small particles, either resting on a surface or optically trapped at a laser focus, where the confocal collection volume optimizes the signal from the particle. In this work, the sensitivity and spatial selectivity of detecting Raman scattering from single particles was determined as a function of particle size. An inverted confocal Raman microscope was used to acquire spectra of individual surface-bound and optically trapped polystyrene particles with sizes ranging between 200 nm and 10 microm. The particles are in contact with aqueous solution containing perchlorate ion that served as a solution-phase Raman-active probe to detect interferences from the surrounding medium. The collection volume is scanned through single particles that are attached to the surface of the coverslip, and the sensitivity and selectivity of detection are measured versus particle size. The results compare favorably with a theoretical analysis of the excitation profile and confocal collection efficiency integrated over the volumes of the spherical particles and the surrounding solution. This analysis was also applied to the detection of particles that are optically trapped and levitated above the surface of the coverslip. The results are consistent with the optical trapping of particles at or near the excitation beam focus, which optimizes excitation and selective collection of Raman scattering from the particle.     

同步辐射白光形貌术观察SiC单晶中的微小多型结构

采用同步辐射白光形貌术观察了6H和4H-SiC单晶片中的微小多型结构.基于透射同步辐射形貌术的衍射几何和晶片的取向,计算了SiC晶体中3种主要多型在Lane像中对应不同反射的成像位置,并与实际结果进行了比较.鉴别出6H和4H-SiC单晶中分别存在着少量的4H-SiC和15R-SiC多型的寄生生长.     

Femtosecond electron beam generation and measurement for laser synchrotron radiation

One of the S-band twin linacs (18L linac) of Nuclear Engineering Research Laboratory of University of Tokyo is modified in order to produce femtosecond electron single bunch for femtosecond X-ray generation via Thomson backward scattering, namely laser synchrotron radiation. Laser photocathode RF gun and chicane-type magnetic pulse compressor are installed at the S-band linac. 10 ps (FWHM) laser pulse generates 5 MeV, 10 ps (FWHM), 1 nC electron single bunch, which is accelerated up to 20 MeV in the S-band accelerating tube and compressed to 200 fs (FWHM) by the chicane. Design study has been performed by using the code of PARMELA and the installation has been finished. For precise and reliable measurement of the compressed pulse length, the comparison of measurement between the femtosecond streak camera and coherent transition radiation interferometry was carried out. Good agreement between them for 1-10 ps (FWHM) pulses was achieved. A new Michelson interferometer for the 200 fs pulse is now under construction.     

Gas thermodynamics and optics of a monodisperse supersonic jet interacting with an aerodynamic body

On the basis of the previously developed gas dynamics model of the polydisperse jet flowing over a blunt body, the optics of a compressed layer is studied under close-to-experimental conditions. The effect of scattering of monochromatic radiation by the particles on the observed picture in the ??laser sheet?? plane is numerically estimated. The study is carried out on the assumption that the cloud formed by the particles is optically thin (single scattering). The effects of absorption and scattering of the radiation by the carrying gas are neglected. The numerical studies have been carried out for wide ranges of the particle sizes and optical parameters of the matter.     

同步辐射小角X射线散射及其在材料研究中的应用

小角X射线散射(small angle X-ray scattering,SAXS)是研究物质内部一纳米到数百纳米甚至到微米尺度级别微观结构的有力工具.近年来随着我国同步辐射技术的不断发展,同步辐射SAXS技术被越来越多地应用到各种材料的研究领域.然而,由于SAXS图谱是倒空间的信号,并不像显微镜那么直观,也不如X射线...     

Absolute distance measurement of optically rough objects using asynchronous-optical-sampling terahertz impulse ranging

We report on a real-time terahertz (THz) impulse ranging (IPR) system based on a combination of time-of-flight measurement of pulsed THz radiation and the asynchronous-optical-sampling (ASOPS) technique. The insensitivity of THz radiation to optical scattering enables the detection of various objects having optically rough surfaces. The temporal magnification capability unique to ASOPS achieves precise distance measurements of a stationary target at an accuracy of -551 μm and a resolution of 113 μm. Furthermore, ASOPS THz IPR is effectively applied to real-time distance measurements of a moving target at a scan rate of 10 Hz. Finally, we demonstrate the application of ASOPS THz IPR to a shape measurement of an optically rough surface and a thickness measurement of a paint film, showing the promise of further expanding the application scope of ASOPS THz IPR. The reported method will become a powerful tool for nondestructive inspection of large-scale structures.     

Synthesis and structure of large single crystalline silver hexagonal microplates suitable for micromachining

We report a simple one-step synthesis method of large single crystalline Ag (111) hexagonal microplates with sharp edges and a size of up to tens of microns. Single silver crystals were produced by reduction silver nitrate aqueous solution with 4-(methylamino)phenol sulfate. Scanning and transmission electron microscopy, energy-dispersive X-ray spectroscopy, selected area electron diffraction and optical microscopy techniques were combined to characterize the crystals. It is shown that the microplates can be easily dispersed and transferred as single objects onto different substrates and subsequently used as a high quality plasmonic starting material for micromachining of future nanocomponents, using modern top-down techniques like focused-ion beam milling and gas injection deposition.     

Simulation studies of atomic resolution X-ray holography

X-ray holography is a new method of structure determination based on measurement of interference of a known reference wave with an unknown object wave (containing information on atomic sites scattering the reference wave) so that phase information is preserved. Unlike X-ray diffraction, it does not demand for translational periodicity in the material. It is based on the idea similar to that of optical holography and has been tested on crystals, quasicrystals, thin films and doped semiconductors for their structure determination. In order to analyse potentials and limitations of this technique, we have carried out theoretical simulation studies on simple structures. In this paper we describe the basic algorithm of hologram generation and reconstruction of atomic positions from generated data. We illustrate this technique using Fe (bcc) single crystal as sample case to demonstrate its capabilities and limitations. Simulations were carried out on the Cu (fcc) structure and on complex structure such as the Al-Pd-Mn quasicrystal. Technical issues such as low signal to noise ratio, twin image problem etc have been discussed briefly to emphasize the need for high intensity X-ray source such as synchrotron for experiments and proper reconstruction algorithm. Finally the scope and potential of this technique have been discussed.     

Measurement of the surface profile of a curved optical surface with rotation phase-shifting lateral shear cyclic path optical configuration

We present a new (to our knowledge) technique for introducing phase shifts between the laterally sheared emergent beam components of a cyclic path optical configuration (CPOC). The phase shifts are introduced by applying a small change in the angle of incidence of the incident beam due to the small angular rotation of the CPOC setup. Phase-shifting interferometry has been applied along with this phase-shifting technique for a CPOC with lateral shear to find the surface slope/profile of curved optical surfaces. Results for a spherical optical surface have been discussed. An optical setup for measurement of the surface profile of toroidal beam line mirrors of synchrotron radiation sources is proposed.     

An investigation of mortars affected by alkali-silica reaction by X-ray synchrotron microtomography: a preliminary study

A first attempt to investigate samples affected by alkali-silica reaction (ASR) by synchrotron X-ray microtomography has been made. The setup available at the SYRMEP beamline, at the third generation synchrotron Elettra (Trieste, Italy), allowed collecting phase-contrast enhanced images, with a detectability approaching that of optical microscopy (a few microns). In this study, mortar cylinders were prepared and immersed in a 1-M NaOH solution at 80 °C for 14 days to enhance the ASR. The weathered samples were studied using the traditional 2D techniques such as optical microscopy and scanning electron microscopy as well as using the 3D micro-CT. Over the aged samples, the 3D imaging allows the ASR weathering to be studied, showing the reactive aggregate progressive dissolution with subsequent deposition of gel and microcracks development. This technique has proven to be a valuable, non-destructive, method which allows the rendering of the microstructural features in specimen affected by ASR.