Quantitative phase retrieval in X‐ray Zernike phase contrast microscopy

In recent years, increasing attention has been devoted to X‐ray phase contrast imaging, since it can provide high‐contrast images by using phase variations. Among the different existing techniques, Zernike phase contrast microscopy is one of the most popular phase‐sensitive techniques for investigating the fine structure of the sample at high spatial resolution. In X‐ray Zernike phase contrast microscopy, the image contrast is indeed a mixture of absorption and phase contrast. Therefore, this technique just provides qualitative information on the object, which makes the interpretation of the image difficult. In this contribution, an approach is proposed for quantitative phase retrieval in X‐ray Zernike phase contrast microscopy. By shifting the phase of the direct light by π/2 and 3π/2, two images of the same object are measured successively. The phase information of the object can then be quantitatively retrieved by a proper combination of the measured images. Numerical experiments were carried out and the results confirmed the feasibility of the proposed method. It is expected that the proposed method will find widespread applications in biology, materials science and so on.     

Current status of the TwinMic beamline at Elettra: a soft X‐ray transmission and emission microscopy station

The current status of the TwinMic beamline at Elettra synchrotron light source, that hosts the European twin X‐ray microscopy station, is reported. The X‐ray source, provided by a short hybrid undulator with source size and divergence intermediate between bending magnets and conventional undulators, is energy‐tailored using a collimated plane‐grating monochromator. The TwinMic spectromicroscopy experimental station combines scanning and full‐field imaging in a single instrument, with contrast modes such as absorption, differential phase, interference and darkfield. The implementation of coherent diffractive imaging modalities and ptychography is ongoing. Typically, scanning transmission X‐ray microscopy images are simultaneously collected in transmission and differential phase contrast and can be complemented by chemical and elemental analysis using across‐absorption‐edge imaging, X‐ray absorption near‐edge structure or low‐energy X‐ray fluorescence. The lateral resolutions depend on the particular imaging and contrast mode chosen. The TwinMic range of applications covers diverse research fields such as biology, biochemistry, medicine, pharmacology, environment, geochemistry, food, agriculture and materials science. They will be illustrated in the paper with representative results.     

Hollow glass microspheres coated with CoFe2O4 and its microwave absorption property

Spinel CoFe₂O₄ coating on the surface of hollow glass microspheres of low density was synthesized by co-precipitation method. The phase structures, morphologies, particle size, shell thickness, chemical compositions of the composites have been characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM) and energy dispersive X-ray spectroscopy (EDS). The results show that CoFe₂O₄ coating on hollow glass microspheres can be achieved, and the coating layers are constituted by CoFe₂O₄ nanoparticles of mean size ca. 10 nm. The as-synthesized powder materials were uniformly dispersed into the phenolic cement, then the mixture was pasted on metal plate with the area of 200 mm×200 mm as the test plate. The test of microwave absorption was carried out by the radar-absorbing materials (RAM) reflectivity far field radar cross-section (RCS) method. The results indicate that the coated CoFe₂O₄/hollow glass microspheres composites can be applied in lightweight and strong absorption microwave absorbers.     

X‐ray analyzer‐based phase‐contrast computed laminography

X‐ray analyzer‐based phase‐contrast imaging is combined with computed laminography for imaging regions of interest in laterally extended flat specimens of weak absorption contrast. The optics discussed here consist of an asymmetrically cut collimator crystal and a symmetrically cut analyzer crystal arranged in a nondispersive (+, ?) diffraction geometry. A generalized algorithm is given for calculating multi‐contrast (absorption, refraction and phase contrast) images of a sample. Basic formulae are also presented for laminographic reconstruction. The feasibility of the method discussed was verified at the vertical wiggler beamline BL‐14B of the Photon Factory. At a wavelength of 0.0733 nm, phase‐contrast sectional images of plastic beads were successfully obtained. Owing to strong circular artifacts caused by a sample holder, the field of view was limited to about 6 mm in diameter.     

Plasma sprayed alumina coatings for radiation detector development

Conventional design of radiation detectors uses sintered ceramic insulating modules. The major drawback of these ceramic components is their inherent brittleness. Ion chambers, in which these ceramic spacers are replaced by metallic components with plasma spray coated alumina, have been developed in our Research Centre. These components act as thin spacers that have good mechanical strength as well as high electrical insulation and replace alumina insulators with the same dimensions. As a result, the design of the beam loss monitor ion chamber for CAT could be simplified by coating the outer surface of the HT electrode with alumina. One of the chambers developed for isotope calibrator for brachytherapy gamma sources has its outer aluminium electrode (60 mm dia × 220 mm long) coated with 250 μ thick alumina (97%) + titania (3%). In view of potential applications in neutron-sensitive ion chambers used in reactor control instrumentation, studies were carried out on alumina 100 μ to 500 μ thick coatings on copper, aluminium and SS components. The electrical insulation varied from 10⁸ ohms to 10¹² ohms for coating thicknesses above 200 μ. The porosity in the coating resulted in some fall in electrical insulation due to moisture absorption. An improvement could be achieved by providing the ceramic surface with moisture-repellent silicone oil coating. Irradiation at Apsara reactor core location showed that the coating on aluminium was found to be unaffected after exposure to 10¹⁷ nvt fluence.     

Vanadium carbide coatings on die steel deposited by the thermo-reactive diffusion technique

Thermal reactive diffusion coating of vanadium carbide on DIN 1.2367 die steel substrate was performed in a powder mixture consisting of ferro-vanadium, ammonium chloride, alumina and naphthalene at 950, 1050 and 1150 °C for 1-5 h. The carbide layers were characterized by means of microstructure, microhardness, X-ray diffraction and chemical analysis. Depending on the coating process time and temperature, the thickness of the vanadium carbide layer formed on the substrate ranged from 2.3 to 23.2 μm. The hardness of vanadium carbide layers was about 2487 HV. Dry wear tests for uncoated and coated DIN 1.2367 die steel were carried out on pin-on-disk configuration and at a sliding speed of 0.13 m/s. The results showed superior wear properties of the coated samples. The kinetics of vanadium carbide coating by the pack method was also studied and the activation energy for the thermo-reactive diffusion process was estimated to be 173.2 kJ/mol.     

衍射增强成像提取多种信息的简便方法研究

衍射增强相位衬度成像中的信息分离研究一直以来都是相关研究人员重点关注的方向之一. 本文在利用余弦函数拟合衍射增强成像中的摇摆曲线的基础上, 推导出了峰位像、左腰像和右腰像的余弦函数表达式以及吸收像、折射角像和散射角方差像的解析表达式, 形成了一种基于衍射增强成像的简便信息分离方法. 该方法只需利用摇摆曲线左腰、右腰和峰位三幅图像, 就能提取出样品的吸收、折射和散射信息, 具有方法简便、样品所受辐射剂量低等优点. 对模型样品和真实样品的实验结果表明, 本文所提方法可成功对样品进行信息分离, 并且所获得的信息分离结果可以和目前常用的多图统计方法(至少需要7张图像)获得的实验结果相比较. 关键词： 衍射增强成像 相位衬度成像 样品信息提取     

X‐ray grating interferometer for biomedical imaging applications at Shanghai Synchrotron Radiation Facility

An X‐ray grating interferometer was installed at the BL13W beamline of Shanghai Synchrotron Radiation Facility (SSRF) for biomedical imaging applications. Compared with imaging results from conventional absorption‐based micro‐computed tomography, this set‐up has shown much better soft tissue imaging capability. In particular, using the set‐up, the carotid artery and the carotid vein in a formalin‐fixed mouse can be visualized in situ without contrast agents, paving the way for future applications in cancer angiography studies. The overall results have demonstrated the broad prospects of the existing set‐up for biomedical imaging applications at SSRF.     

Feasibility study of propagation‐based phase‐contrast X‐ray lung imaging on the Imaging and Medical beamline at the Australian Synchrotron

Propagation‐based phase‐contrast X‐ray imaging (PB‐PCXI) using synchrotron radiation has achieved high‐resolution imaging of the lungs of small animals both in real time and in vivo. Current studies are applying such imaging techniques to lung disease models to aid in diagnosis and treatment development. At the Australian Synchrotron, the Imaging and Medical beamline (IMBL) is well equipped for PB‐PCXI, combining high flux and coherence with a beam size sufficient to image large animals, such as sheep, due to a wiggler source and source‐to‐sample distances of over 137 m. This study aimed to measure the capabilities of PB‐PCXI on IMBL for imaging small animal lungs to study lung disease. The feasibility of combining this technique with computed tomography for three‐dimensional imaging and X‐ray velocimetry for studies of airflow and non‐invasive lung function testing was also investigated. Detailed analysis of the role of the effective source size and sample‐to‐detector distance on lung image contrast was undertaken as well as phase retrieval for sample volume analysis. Results showed that PB‐PCXI of lung phantoms and mouse lungs produced high‐contrast images, with successful computed tomography and velocimetry also being carried out, suggesting that live animal lung imaging will also be feasible at the IMBL.     

Design,development and first experiments on the X‐ray imaging beamline at Indus‐2 synchrotron source RRCAT,India

A full‐field hard X‐ray imaging beamline (BL‐4) was designed, developed, installed and commissioned recently at the Indus‐2 synchrotron radiation source at RRCAT, Indore, India. The bending‐magnet beamline is operated in monochromatic and white beam mode. A variety of imaging techniques are implemented such as high‐resolution radiography, propagation‐ and analyzer‐based phase contrast imaging, real‐time imaging, absorption and phase contrast tomography etc. First experiments on propagation‐based phase contrast imaging and micro‐tomography are reported.     

Microwire formation based on dielectrophoresis of electroless gold plated polystyrene microspheres

Microspheres coated with a perfectly conductive surface have many advantages in the applications of biosensors and micro-electromechanical systems.Polystyrene microspheres with the diameter of 10 μm were coated with a 50 nmthick gold layer using an electroless gold plating approach.Dielectrophoresis(DEP) for bare microspheres and shelled microspheres was theoretically analysed and the real part of the Clausius-Mossotti factor was calculated for the two kinds of microspheres.The experiments on the dielectrophoretic characterisation of the uncoated polystyrene microspheres and gold coated polystyrene microspheres(GCPMs) were carried out.Experimental results showed that the gold coated polystyrene microspheres were only acted by a positive dielectrophoretic force when the frequency was below 40M Hz,while the uncoated polystyrene microspheres were governed by a negative dielectrophoretic force in this frequency range.The gold coated polystyrene microspheres were exploited to form the microwire automatically according to their stable dielectrophoretic and electric characterisations.     

Advanced phase‐contrast imaging using a grating interferometer

Phase‐sensitive X‐ray imaging methods can provide substantially increased contrast over conventional absorption‐based imaging, and therefore new and otherwise inaccessible information. Differential phase‐contrast (DPC) imaging, which uses a grating interferometer and a phase‐stepping technique, has been integrated into TOMCAT, a beamline dedicated to tomographic microscopy and coherent radiology experiments at the Swiss Light Source. Developments have been made focusing on the fast acquisition and post‐processing of data to enable a high‐throughput of samples, with obvious advantages, also through increasing the efficiency of the detecting system, of helping to reduce radiation dose imparted to the sample. A novel aquarium design allows a vertical rotation axis below the sample with measurements performed in aqueous environment. Optimization of the data acquisition procedure enables a full phase volume (1024 × 1024 pixels × 1000 projections × 9 phase steps, i.e. 9000 projections in total) to be acquired in 20 min (with a pixel size of 7.4 µm), and the subsequent post‐processing has been integrated into the beamline pipeline for sinogram generation. Local DPC tomography allows one to focus with higher magnification on a particular region of interest of a sample without the presence of local tomography reconstruction artifacts. Furthermore, `widefield' imaging is shown for DPC scans for the first time, enabling the field of view of the imaging system to be doubled for samples that are larger than the magnification allows. A case study is illustrated focusing on the visualization of soft tissue features, and particularly the substantia nigra of a rat brain. Darkfield images, based on local X‐ray scattering, can also be extracted from a grating‐based DPC scan: an example of the advantages of darkfield contrast is shown and the potential of darkfield X‐ray tomography is discussed.     

Evolution mechanism of alumina coating layer on rutile TiO2 powders and the pigmentary properties

The evolution of alumina coating layers on rutile TiO₂ particle surfaces was investigated starting from aluminum sulfate by a chemical liquid deposition method. The morphology of the alumina coating layers was determined by transmission electron microscopy. The chemical structure and the evolution mechanism of the alumina coating layers on TiO₂ surfaces were investigated by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and powder X-ray diffraction techniques. The dispersibility of the alumina-coated TiO₂ powders was determined by dynamic laser scattering (DLS) mode. The alumina coating layers existed in boehmite phase, AlOOH, and anchored at the surfaces of TiO₂ via Ti-O-Al bond. The formation of alumina coating layers on TiO₂ surfaces depended on the pH value of the deposition solution and the alumina loading. After coated by alumina layer, the dispersibility, whiteness, brightness, and light scattering index of the resultant samples were promoted.     

Investigations on composition and morphology of electrochemical alumina and alumina–yttria stabilised zirconia deposits

Conversion coatings modified by deposits of electrolytic alumina added or not with yttria and/or zirconia, have been studied which are well known for their resistance to chemical attack and high temperature. Conversion coating, characterised by a particular morphology and strong interfacial adhesion with the substrate, facilitate the electrochemical deposition of ceramic layers and enhance their adhesion to the substrate. Zirconia–alumina coating behaviour at 1000°C is similar to that of alumina coating; from 800°C, the chromium diffuses from the stainless steel through the electrolytic refractory coating up to the external interface, provokes discontinuities and can modify its protective character. Yttrium stabilises the cubic and the tetragonal form of the zirconia; so, during cooling, the phase transformation near 1000°C of tetragonal zirconia to monoclinic form cannot take place.     

Effects of volatile coatings on the laser-induced incandescence of soot

We have measured time-resolved laser-induced incandescence (LII) from combustion-generated mature soot extracted from a burner and (1) coated with oleic acid or (2) coated with oleic acid and then thermally denuded using a thermodenuder. The soot samples were size selected using a differential mobility analyzer and characterized with a scanning mobility particle sizer, centrifugal particle mass analyzer, and transmission electron microscope. The results demonstrate a strong influence of coatings on the magnitude and temporal evolution of the LII signal. For coated particles, higher laser fluences are required to reach signal levels comparable to those of uncoated particles. The peak LII curve is shifted to increasingly higher fluences with increasing coating thickness until this effect saturates at a coating thickness of ~75 % by mass. These effects are predominantly attributable to the additional energy needed to vaporize the coating while heating the particle. LII signals are higher and signal decay rates are significantly slower for thermally denuded particles relative to coated or uncoated particles, particularly at low and intermediate laser fluences. Our results suggest negligible coating enhancement in absorption cross-section for combustion-generated soot at the laser fluences used. Apparent enhancement in absorption with restructuring may be caused by less conductive cooling.     

无吸收光栅的X射线相位衬度成像实验研究

通过对基于空间相干源和具有分析光栅功能的X射线转换屏的微分干涉X射线相位衬度成像 系统的理论分析, 利用线发射体阵列结构阳极X射线管和光助电化学刻蚀技术 研制的相位光栅和具有分析光栅功能的X射线转换屏, 组建了一种无吸收光栅的X射线微分干涉相衬成像系统. 在此系统上开展了生物样品的实验研究, 获得了较传统吸收成像更为清晰和更多样品结构信息的相位衬度图像. 从而试验验证了该系统方案设计的可行性, 为X射线相衬成像技术从实验室走向临床应用提供了有效途径.     

X‐ray microtomographic visualization of Escherichia coli by metalloprotein overexpression

This paper reports X‐ray microtomographic visualization of the microorganism Escherichia coli overexpressing a metalloprotein ferritin. The three‐dimensional distribution of linear absorption coefficients determined using a synchrotron radiation microtomograph with a simple projection geometry revealed that the X‐ray absorption was homogeneously distributed, suggesting that every E. coli cell was labeled with the ferritin. The ferritin‐expressing E. coli exhibited linear absorption coefficients comparable with those of phosphotungstic acid stained cells. The submicrometer structure of the ferritin‐expressing E. coli cells was visualized by Zernike phase contrast using an imaging microtomograph equipped with a Fresnel zone plate. The obtained images revealed curved columnar or bunching oval structures corresponding to the E. coli cells. These results indicate that the metalloprotein overexpression facilitates X‐ray visualization of three‐dimensional cellular structures of biological objects.     

Raman micro‐spectroscopy for quantitative thickness measurement of nanometer thin polymer films

The sensitivity of far‐field Raman micro‐spectroscopy was investigated to determine quantitatively the actual thickness of organic thin films. It is shown that the thickness of organic films can be quantitatively determined down to 3 nm with an error margin of 20% and down to 1.5 nm with an error margin of 100%. Raman imaging of thin‐film surfaces with a far‐field optical microscope establishes the distribution of a polymer with a lateral resolution of ~400 nm and the homogeneity of the film. Raman images are presented for spin‐coated thin films of polysulfone (PSU) with average thicknesses between 3 and 50 nm. In films with an average thickness of 43 nm, the variation in thickness was around 5% for PSU. In films with an average thickness of 3 nm for PSU, the detected thickness variation was 100%. Raman imaging was performed in minutes for a surface area of 900 µm². The results illustrate the ability of far‐field Raman microscopy as a sensitive method to quantitatively determine the thickness of thin films down to the nanometer range. Copyright © 2015 John Wiley & Sons, Ltd.     

Application of arc-plasma discharges to coating of screw taps

The paper reports on results of technological research on the coating of standard screw taps with TiN layers deposited by means of arc-plasma discharges, which were carried out within a BULAT-type device equipped with three identical metal-plasma sources. Particular attention is paid to morphology of the coated surfaces. Some data about thickness and microhardness of the coating layers, as well as results of laboratory wear tests of the coated tools, are also presented.     

A new method for information retrieval in two-dimensional grating-based X-ray phase contrast imaging

Grating-based X-ray phase contrast imaging has been demonstrated to be an extremely powerful phase-sensitive imaging technique.By using two-dimensional(2D) gratings,the observable contrast is extended to two refraction directions.Recently,we have developed a novel reverse-projection(RP) method,which is capable of retrieving the object information efficiently with one-dimensional(1D) grating-based phase contrast imaging.In this contribution,we present its extension to the 2D grating-based X-ray phase contrast imaging,named the two-dimensional reverseprojection(2D-RP) method,for information retrieval.The method takes into account the nonlinear contributions of two refraction directions and allows the retrieval of the absorption,the horizontal and the vertical refraction images.The obtained information can be used for the reconstruction of the three-dimensional phase gradient field,and for an improved phase map retrieval and reconstruction.Numerical experiments are carried out,and the results confirm the validity of the 2D-RP method.