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The use of non-local self-similarity prior between image blocks can improve image reconstruction performance significantly. We propose a compressive sensing image reconstruction algorithm that combines bilateral total variation and nonlocal low-rank regularization to overcome over-smoothing and degradation of edge information which result from the prior reconstructed image. The proposed algorithm makes use of the preservation of image edge information by bilateral total variation operator to enhance the edge details of the reconstructed image. In addition, we use weighted nuclear norm regularization as a low-rank constraint for similar blocks of the image. To solve this convex optimization problem, the Alternating Direction Method of Multipliers (ADMM) is employed to optimize and iterate the algorithm model effectively. Experimental results show that the proposed algorithm can obtain better image reconstruction quality than conventional algorithms with using total variation regularization or considering the nonlocal structure of the image only. At 10% sampling rate, the peak signal-to-noise ratio gain is up to 2.39 dB in noiseless measurements compared with Nonlocal Low-rank Regularization (NLR-CS). Reconstructed image comparison shows that the proposed algorithm retains more high frequency components. In noisy measurements, the proposed algorithm is robust to noise and the reconstructed image retains more detail information.

With the popularization of automounting robots in protein crystal diffraction experiment beamline stations, the coordinate calibration of the robot sample mounting position has become an inevitable task in the daily maintenance of the beamline station. In this method, the image features of the laser sensor spot and goniometer are extracted by color extraction and edge detection, respectively, and the noise is eliminated by median filtering. Then, after locating the pixel coordinates of the center of the circle through the Hough circle detection and the minimum closed circle fitting algorithm, the coordinates in the base coordinate system are obtained using the camera internal and external parameter matrices and the hand-eye relationship matrix. Finally, according to the deviation of the laser spot and the visual positioning coordinate of the goniometer, the position of the robot is compensated to improve the positioning accuracy, and the automatic calibration of the sample point is realized.

Double-ReO3-type structure compound NaSbF6 undergoes a low-temperature rhombohedral to high-temperature cubic phase between 303 and 323 K, as revealed by temperature-dependent X-ray diffractions. Although many double-ReO3-type fluorides exhibit either low thermal expansion or negative thermal expansion (NTE), NaSbF6 exhibits positive thermal expansion (PTE) with a large volumetric coefficient of thermal expansion, αv = 62 ppm/K, in its cubic phase. Raman spectroscopy reveals that the low-frequency transverse vibration of fluorine atoms is stiffened in NaSbF6, compared with the typical NTE compound CaZrF6 with the same structure. The related weak contraction associated with the polyhedral rocking would be overcome by the notable elongation of the Na–F bond length on heating, thus leading to the large volumetric PTE. Unlike ScF3 and CaZrF6 which are insulators with a wide band gap, a relative small band gap of 3.76 eV was observed in NaSbF6. The small band gap can be attributed to the hybridization between ...

As the Mn doping level ( x ) increases in cubic (Ga 0.7 Cu 0.3 ) 1- x Mn x NMn 3 ( x ≤ 0.4) compounds, the temperature window of negative thermal expansion (NTE) is shifted to lower temperatures and broadened due to the strengthening of ferromagnetism. Large coefficient of linear thermal expansion ( α ~ − 22.8 ppm/K) is observed for x = 0.25 and 0.3 at cryogenic temperatures ( x = 0.3 powders, the thermal expansion of epoxy resin is effectively reduced. Nearly zero thermal expansion ( α ~ 1 ppm/K) and remarkably improved thermal conductivity are achieved at cryogenic temperatures in the composite with 50 vol.% addition of the NTE filler.

First principle calculations are performed to study the interfacial photoelectric properties of Ag n /Bi 2 WO 6 (0 0 1) ( n = 1, 2, 3, 4) hybrid photocatalyst. The parallel adsorption of Ag cluster leads to more energetic favorable structures due to stronger interfacial interactions. The positive charged Ag cluster may act as excited electron traps and facilitate the electron⿿hole separation. In particular, hybridization between Ag 5s and O 2p leads to the formation of isolated energy levels above the valence bands, and they become more dispersed with broader bandwidth with the increment of silver cluster size, which is responsible for the enhanced absorption in visible-light region. In the deep valence region, Ag 4d orbital turns more delocalized and hybrid with O 2p states as the cluster size increases, which contributes to more covalent bond feature of Ag⿿O. Moreover, optical spectra demonstrate obvious red-shifts of the absorption edge with the increment of silver content, which enhances efficiently the visible-light photocatalytic activities of Bi 2 WO 6 (0 0 1). The study provides insights into the enhanced photocatalyic mechanism of Ag/Bi 2 WO 6 (0 0 1) and aids in the design of noble metal loaded visible-light plasmonic photocatalyst.

Beamline BL17U1 at Shanghai Synchrotron Radiation Facility is an energy-tunable macromolecular crystallography beamline that has been in user operation since 2009. Growing demand from the user community for a small beam and related experimental methods have motivated upgrades of the devices in the endstation. Minibeam modes have already been developed for operation. A self-integrated diffractometer reduces the sphere of confusion of the rotatory axis to 1 µm. The new diffractometer is equipped with an upgraded on-axis viewing system that can improve the resolving power. Additionally, the area detector was also upgraded to the newest generation of detectors, the EIGER X 16M, which can collect data at 133 Hz. After these upgrades, the endstation became virtually new. This paper covers the upgrade of the endstation devices and gives the first data collection results.

Herein, β-Bi2O3 nanosheets exposed with active {001} facets were facilely prepared through annealing Bi2O2CO3 with thermally stable {001} facets. The enhanced photocatalytic activity of β-Bi2O3 was ascribed to the high energy of {001} facets and the efficient charge separation. This 2D surface transformation strategy could shed new light on the fabrication of energetic facets and the development of highly active photocatalysts.

National audience; Background: X-ray position sensitive detector is indispensable for beamlines at synchrotron radiation facilities. Synthetic single-crystal diamond position sensitive detectors have been developed to take advantage of next-generation synchrotron sources, which are trending toward use of high-flux beams and/or beams requiring enhanced stability and precise understanding of beam position and intensity from the front end of the beamline all the way to the sample in recent years. Purpose: It is aimed to provide accurate real-time position and flux for high-flux X-ray beams. Methods: Based on the principle of potentiometers, the transmission-mode diamond X-ray position sensitive detector works as a “solid” ionization chamber. When the X-ray beam comes into the detector’s sensitive region, electronic-holes occur due to the effect of ionization and the charges or the current pulses on the electrodes of the detector are given. According to the collected currents on the electrodes, the location of the incident X-ray can be determined by the ratio between the current difference of electrodes and the total current. Results: A signal/noise ratio of (S/N)>5×10³ and a position resolution of σ=(136±11) nm for the synthetic single-crystal diamond position sensitive detector with an active area of 2.5 mm×2.5 mm, respectively, have been obtained. The measurement precisions for the X-ray beam intensity and position linearity are less than 0.1%. Conclusion: We have demonstrated the feasibility of building a transmission-mode synthetic single-crystal diamond X-ray position sensitive detector, which could measure X-ray beam intensity and position in real time. Its performance was determined on the macromolecular crystallography beamline (BL17U1) at SSRF. Experimental data show that the diamond detector has good linear response and measurement precision of beam intensity within the whole active area.

The protein elicitor from Alternaria tenuissima (PeaT1) presented excellent thermotolerance and potential application in agriculture as a pesticide. Previous synchrotron radiation circular dichroism study demonstrated that the secondary structures in PeaT1 protein are reversible with temperature change. To further clarify the mechanism of its thermotolerance, synchrotron radiation small angle x-ray scattering (SAXS) technique was used to study the shape change of PeaT1 protein with temperature in this article. Ab initio structure restorations based on the SAXS data revealed that PeaT1 protein has a prolate shape with a P2 symmetry axis along the prolate anisometric direction. With temperature increase, a gooseneck vase-like (25 degrees C), to jug-like (55 degrees C), then to oval (85 degrees C) shape change can be found, and these shape changes are also approximately reversible with temperature decrease. PeaT1 protein contains two homogenous molecules, and each of them consists of F, NAC, T, and UBA domains. The structures of the four domains were predicted. Simulated annealing algorithm was used to superimpose the domain structures onto the SAXS shapes. It was found that all the structural domains have position rotation and translation with temperature change, but the NAC domains are relatively stable, playing a role of frame. This shape change information provides clues for further exploring its biological function and application. Proteins 2013. (c) 2012 Wiley Periodicals, Inc.

Wood is a highly sophisticated and multihierarchical material. The nanoscale structures in natural cell walls of red pine, American pine, and white ash specimens were investigated using the small-angle X-ray scattering (SAXS) technique. A tangent-by-tangent method was used to analyze the SAXS data. The results demonstrate that the multihierarchical scatterers in the three specimens can be divided into two dominant components, i.e., a sharp component and a wide component. The sharp component mainly corresponds to the contribution of cellulose microfibrils, and its size is almost unaffected by the water content. However, the wide component includes voids or microcracks and cellulose microfibril aggregates; its size changes, reflecting swelling and water accumulation in the voids or microcracks. Because of the different morphological features of the cell walls, softwood (red pine and American pine) displays different tendencies from hardwood (white ash) in terms of changes in the wide component with water content: the average scatterer size of the wide component has an incremental tendency with the water content in softwood, but it has a descending tendency in hardwood. Fractal analysis further revealed that in white ash the surface of scatterers is coarser and the scatterers form more compact nanostructures than in the two pine woods. All this nanostructural information can be used to explain well the difference of swelling behaviors between the two pines and the white ash.

Gold nanoparticles were synthesized with seed mediated wet growth method. A coexistent system with gold nanorods and nanospheres was prepared. In-situ real-time small angle X-ray scattering (SAXS) and ultraviolet-visible (UV-vis) absorption were used to monitor the growth process of Au nanoparticles in the aqueous solution. Combining SAXS measurement and UV-vis spectra, the contribution of gold nanorods was separated from that of gold nanospheres. The growth behavior of the gold nanorods and the gold nanospheres was studied. The size and shape evolution of both gold nanoparticles as well as their volume fractions were obtained. After adding the seed-solution into the growth solution to form a particle suspension, within the first 18 min, a mutual competitive growth occurred between the gold nanorods and nanospheres. And their average particle sizes always increased with growth time. 18-min later, the evolution of size and shape of gold nanoparticles was almost stopped. The results demonstrate that the aspect ratio of gold nanorods in the particle suspension follows an exponential decay change after the initial 5-min growth. The evolution process of size and shape of gold nanoparticles in the particle suspension has been discussed.

Ni–Cu alloy nanowire array, with uniform length and diameter, was well fabricated by using alternating current electrodeposition. Both X-ray diffraction and in situ heating extended X-ray absorption fine structure technique were employed to characterize its structural change with temperature. As expected, a weak concentration fluctuation of Ni and Cu atoms was found in the as-prepared nanowires. However, this concentration fluctuation can be easily eliminated by heating the as-prepared sample at 200 °C, which resulting in an approximately homogeneous Ni–Cu solid solution. From the nanostructural point of view, the serviceability temperature of Ni–Cu alloy nanowire array in magnetism could not exceed 200 °C. The Ni–Ni, Ni–Cu and Cu–Cu bonds were found to have different thermal expansion behaviors, causing the distortion of the crystal cell. An average thermal expansion coefficient (1.1 × 10 −5 K −1 ) was obtained. The structural change of Ni–Cu alloy nanowires with temperature was discussed.

The effect of CO(2) on the microstructure of L-alpha-phosphatidylcholine (lecithin) reverse micelles was studied. The small-angle X-ray scattering (SAXS) results show that CO(2) could induce a cylindrical-to-spherical micellar shape transformation. Fourier transform infrared (FT-IR) and UV-vis techniques were also utilized to investigate intermolecular interactions and micropolarity in the reverse micelles at different CO(2) pressures. The reduction of the degree of hydrogen bonding between surfactant headgroups and water with added CO(2) was found to be the main reason for the micellar shape transformation. In the absence of CO(2), the hydrogen bonding between water and P=O of lecithin forms a linking bridge in the interfacial layer. Therefore, the free movement of the polar head of lecithin is limited and the cylindrical reverse micelles are formed. Upon adding CO(2) to the reverse micelles, the hydrogen bonds between lecithin and water in reverse micelles are destroyed, which is favorable to forming spherical micelles. Moreover, the CO(2)-combined reverse micelles were utilized in the synthesis of silica particles. Rodlike silica nanoparticles were obtained in the absence of CO(2), and ellipsoidal and spherical mesoporous silica particles were formed in the presence of CO(2). This method of tuning micellar shape has many advantages compared to traditional methods.

Core−shell nanoparticles were widely studied because of their potential application. However, there are few reports about the interfacial structure and its stability. In this paper, Au@SiO2 nanoparticles have been synthesized by using the traditional sol−gel method. In situ extended X-ray absorption fine structure technique was used to characterize the structural change with temperature. It is found that the interfacial bonding between the Au core and the silica shell has changed from a Au−N bond to a Au−Si bond when the temperature is above 600 °C. The Au−silica interface with Au−Si bonds between the Au core and silica shell can be stably existed in the temperature range of 600 to 1000 °C. The mechanism of bond change is described. The thermal expansion coefficient of Au nanoparticles in the Au@SiO2 core−shell system is obtained to be 1.4 × 10−5 K−1, which is almost the same with Au bulk. The details of the structural changes and thermal expansion behavior are discussed in this paper.

Poly(vinylpyrrolidone) (PVP)-coated platinum (Pt) nanoparticles were prepared in methanol-water reduction method. In situ small-angle X-ray scattering (SAXS) and X-ray diffraction (XRD) techniques were used to probe the size change of particles and crystallites with temperature. Tangent-by-tangent (TBT) method of SAXS data analysis was improved and used to get the particle size distribution (PSD) from SAXS intensity. Scherrer’s equation was used to derive the crystallite size from XRD pattern. Combining SAXS and XRD results, a step-like characteristic of the Pt nanoparticle growth has been found. Three stages (diffusion, aggregation, and agglomeration) can be used to describe the growth of the Pt nanoparticles and nanocrystallites. Aggregation was found to be the main growth mode of the Pt nanoparticles during heating. The maximum growth rates of Pt nanoparticles and Pt nanocrystallites, as well as the maximum aggregation degree of Pt nanocrystallites were found, respectively, at 250 °C, 350 °C and 300 °C. These results are helpful to understanding the growth mode of nanoparticles, as well as controlling the nanoparticle size.

Cubic germanium dioxide (GeO2) nanoparticles coated by sodium bis(2-ethylhexyl) sulfosuccinate (AOT) were synthesized with a reverse micelle technique. In situ heating extended X-ray absorption fine-structure technique was used to investigate the change of the local atomic structure and electronic structure around germanium. A direct formation of Ge−S bond was found from GeO2 at high temperature and ambient pressure. This Ge−S bond was identified to be temperature-dependent. The change of the local structure with heating is discussed. This study provides a routine process to synthesize GeS2 from GeO2 at higher temperature and ambient pressure.

In this paper, the Co@SiO2 core-shell nanoparticles were prepared by the sol-gel method. The oxidization of Co core nanoparticles was studied by the synchrotron radiation-based techniques including in situ X-ray diffraction (XRD) and X-ray absorption fine structure (XAFS) up to 800°C in air and N2 protection conditions, respectively. It was found that the oxidization of Co cores is undergoing three steps regardless of being in air or in N2 protection condition. In the first step ranging from room temperature to 200°C, the Co cores were dominated by Co(0) state as well as small amount of Co(2+) ions. When temperature was above 300°C, the interface between Co cores and SiO2 shells was gradually oxidized into Co(2+), and the CoO layer was observed. As the temperature increasing to 800°C, the Co cores were oxidized to Co3O4 or Co3O4/CoO. Nevertheless, the oxidization kinetics of Co cores is different for the Co@SiO2 in air and N2 gas conditions. Generally, the O2 in the air could get through the SiO2 shells easily onto the Co core surface and induce the oxidization of the Co cores due to the mesoporous nature of the SiO2 shells. However, in N2 gas condition, the O atoms can only be from the SiO2 shells, so the diffusion effect of O atoms in the interface between Co core and SiO2 shell plays a key role.

Polyaniline (PANI)-decorated {001} facets of Bi2O2CO3 nanosheets were synthesized by a low-temperature chemical method. We demonstrate that the strong interfacial interactions between Bi2O2CO3 {001} facets and PANI could promote in situ formation of oxygen vacancy at the interface confirmed by both density functional theory calculations and electron spin resonance experiments, which is due to the high oxygen density characteristic of Bi2O2CO3 {001} facets. In addition, such interfacial interaction also leads to a 0.38 eV positive shifting of the valence band of Bi2O2CO3. Importantly, the decorated PANI can stabilize these interfacial oxygen vacancies. Therefore, the migration and separation of photogenerated carriers have been improved significantly evidenced by electrochemical impedance spectroscopy, photoluminescence, and nanosecond time-resolved fluorescence-decay spectra, resulting in a 4.5 times higher activity toward photodegradation of Rhodamine B and a 6 times higher photocurrent density compared to their corresponding bare Bi2O2CO3. The finding of the in situ oxygen vacancy formation at the interface could provide some hints for the deep understanding of the interactions between PANI and crystal facets of semiconductors to develop highly efficient photocatalysts.

The macromolecular crystallography beamlines at third-generation synchrotron facilities play a central role in solving macromolecular crystal structures and also in understanding the biological function at molecular levels. The MX beamline BL17U at Shanghai Synchrotron Radiation Facility is a typical standard MX beamline with a focused beam size (H × V) of FWHM around 80 μm × 45 μm. However the protein samples brought to the beamline are down to 5-10 m from the important and challenging science project now. These samples require smaller size beam. In order to achieve the mini-size beamline, two mini-beam modes have been developed on BL17U: the pinhole-based mini-beam and the focused mini-beam by compound refractive lens (CRL). Compared to the pinhole-based mode, three times increase in flux is obtained by the CRL mode at a similar beam size. The flux gain obtained by the CRL needs to be considered for data collection strategies. It takes few minutes to switch the beamline from the normal to CRL mini-beam mode.

Normal magnetostriction (MS), which comes from the gradual rotation of magnetic domains in ferromagnets, is anisotropic and smoothly dependent on the applied magnetic field. In cubic antiperovskite compound GaCMn3, a sharp shrink of lattice volume takes place at the antiferromagnetic (AFM) to intermediate magnetic (IM) phase transition. Below the Neel temperature (∼143 K), the AFM-IM transformation can be driven by external magnetic field, leading to a giant isotropic MS of ∼1700 ppm comparable to that of commercial Terfenol-D. In contrast to normal MS, the field-induced magnetostrain exhibits a rapid switch behavior at the critical field. Furthermore, good reversibility and stability were demonstrated for the giant MS of GaCMn3 compound.

Scandium trifluoride (ScF3), adopting a cubic ReO3-type structure at ambient pressure, undergoes a pronounced negative thermal expansion (NTE) over a wide range of temperatures (10 K–1100 K). Here, we report the size effects on the NTE properties of ScF3. The magnitude of NTE is reduced with diminishing the crystal size. As revealed by the specific heat measurement, the low-energy phonon vibrations which account for the NTE behavior are stiffened as the crystal size decreases. With decreasing the crystal size, the peaks in high-energy X-ray pair distribution function (PDF) become broad, which cannot be illuminated by local symmetry breaking. Instead, the broadened PDF peaks are strongly indicative of enhanced atomic displacements which are suggested to be responsible for the stiffening of NTE-related lattice vibrations. The present study suggests that the NTE properties of ReO3-type and other open-framework materials can be effectively adjusted by controlling the crystal size.

Mesostructured germanium oxide has been well-synthesized by using a surfactant-templated approach under basic hydrothermal conditions. The cationic surfactant cetyltrimethylammonium bromide (CTAB) has formed nanotubes with uniform diameter of about 3.2 nm. Blanket-like morphology of the as-prepared sample has been observed with transmission electron microscopy (TEM). High-resolution TEM image reveals that the nanotubes are connected with inorganic germanium oxide and have self-assembled into periodic mesostructure. In-situ heating X-ray diffraction (XRD) patterns confirm that the germanium oxide is in amorphous phase in the temperature range from room temperature (RT) to 700 degrees C. In-situ heating small-angle X-ray scattering (SAXS) presents the mesostructural change with temperature. The local atomic structures around germanium atom have been obtained with in-situ heating X-ray adsorption fine structure (XAFS) techniques. The stability of this mesostructure has been determined to be correlated with the cationic surfactant CTAB. The structural evolution from the GeO 2/NaOH aqueous solution, the as-prepared sample to the sample heated at 700 degrees C, has been described, and the formation mechanism of mesostructured germanium oxide has been discussed.

Electrical transport properties of La2/3Sr1/3VO3 (LSVO) thin films grown on LaAlO3 (LAO) and SrTiO3 (STO) substrates have been investigated. It is found that the LSVO/LAO show metal-insulator transition when decreasing the temperature, while the LSVO/STO exhibit metallic behavior. The difference in transport properties of LSVO thin films has been discussed based on the variation of oxygen content and can be attributed to different oxygen substrate-to-film transfer. These results highlight the crucial role of oxygen stoichiometry in determining the physical properties of LSVO and the importance of oxygen-substrate contribution in LSVO thin films.

A furnace with a water-cooled outside shell has been assembled to do in situ x-ray diffraction (XRD), small angle x-ray scattering (SAXS), and x-ray absorption fine structure (XAFS) experiments. The details of the furnace are described in this paper. The in situ XRD, SAXS, and XAFS experiments during the heating process demonstrate that the available temperature range of this furnace is from room temperature to 1200 K with a temperature accuracy of +/-0.1 K. By using this furnace, in situ XRD, SAXS, and XAFS experimental techniques with temperature change can be easily combined together.

In situ x-ray diffraction and x-ray absorption fine structure techniques were used to study the structural change of ordered Co nanowire array with temperature. The results show that the Co nanowires are polycrystalline with hexagonal close packed structure without phase change up until 700 °C. A nonlinear thermal expansion behavior has been found and can be well described by a quadratic equation with the first-order thermal expansion coefficient of 4.3×10−6/°C and the second-order thermal expansion coefficient of 5.9×10−9/°C. The mechanism of this nonlinear thermal expansion behavior is discussed.