SAXS andalysis of interface in organo—modified mesoporous silica

A small-angle x-ray scattering(SAXS)technique using synchrotron radiation as the x-ray source has been employed to characterize the microstructure of mesoporous silica prepared by one-pot template-directed synthesis methodology.The scattering of pure silica agreed with Porod’s law.the scattering of organomodified mesoporous silica showed a negative deviation from Porod’s law,suggesting that an interfacial layer exists between the pores and silica matrix.It was the organic groups comprising the interface,as shown by ^29Si cross-polarization magic-angle spinning nuclear magnetic resonance imaging (^29Si cp MAS/NMR) and Fourier transform infrared spectroscopy(FTIR),that caused this negative deviation of SAXS intensity from Porod’s law,and the average thichness of the interfacial layer could be deduced from this negative deviation.Copyright 2001 john Wiley and Sons,Ltd.     

Probing new physics in B → J/ψπ~0 decay

We calculate the branching ratio of B → J/ψπ0 with a mixed formalism that combines the QCDimproved factorization and the perturbative QCD approaches.The result is consistent with experimental data.The quite small penguin contribution in B → J/ψπ0 decay can be calculated with this method.We suggest two methods to extract the weak phase β.One is through the dependence of the mixing induced CP asymmetry SJ/ψπ0 on the weak phase β,the other is from the relation of the total asymmetry ACP with the weak phase β.Our results show that the deviation ΔSJ/ψπ0 of the mixing induced CP asymmetry from sin（-2β） is of O（10-3） and has much less uncertainty.The above O（10-3） deviation can provide a good reference for identifying new physics.     

Phase Noise Quenching in a Four-Level Laser

In the presence of usual transmission losses, it is shown that phase noise in a four-level laser can be reduced below the Schawlow-Townes limit when lasing levels are coupled to a squeezed vacuum reservoir. The squeezed vacuum coupled to the lasing mode modifies the phase diffusion rate and dominates the contribution from transmission losses. It is predicted to obtain phase stability in the system and phase noise vanishes for larger squeezing. Gain of the laser remains positive under these conditions.     

Strange—Nonchaotic—Attractor—Like Behaviors in Coupled Map SYstems

In a coupled map system,an attractor which seems to be strange nonchaotic attractor(SNA)is discovered for nonzero measure in parameter range,The attractor has nonpositive Lyapunov exponent(LE) and discrete structure.We call it strange-nonchaotic-attractor-like(SNA-like) behavior because the size of its size of its discrete structure decreases with the computing precision increasing and the true SNA does not change.The SNA-like behavior in the autonomous system is born when the truncation error of round-off is amplified to the size of the discrete part of the attractor during the long time interval of positive local LE.The SNA-like behavior is easily mistaken for a true SNA judging merely from the largest LE and the phase portrait in double precision computing.In non-autonomous system an SNA-like attractor is also found.     

Influence of the randomly varying domain length of quasi—phase—matched crystals on quadrature squeezing performance

During the fabrication of quasi-phase-matched(QPM) devices,errors of periodic structure are usually inevitable.The errors result in the deviation of the actual periodic domain length from the theoretical value.In this paper,we numerically analyse the influence of errors on the quadrature squeezing performance of a degenerate optical parametric amplifier consisting of QPM devices.It is shown that errors significantly degrade the squeezing degree of the quadrature squeezed light.Due to the presence of the errors,the relative phase between the signal and the pump field for obtaining the maximum squezing depends on the propagation distance of light in the crystal and the pump power.     

SCATTERING OF PLANE WAVE BY PIEZOELECTRIC CYLINDER——TRANSFER FUNCTION,TRANSIENT RESPONSES AND PHASE RECONSTRUCTION OF TRANSDUCER

In this paper,under Kirchhoff's assumptions,a theory of the thin shell of radially-Polarizedpiezoelectric ceramic cylinder has been developed.Using the methods of Green's function and separa-tion of variables the scattering of a plane wave by the cylinder has been solved.The normal modeseries expressions of the velocity distribution of the surface of the cylinder and of the total soundfield have been obtained and from those an exact analytic expression of the transfer function of thecylinder as a sound receiver has been give.Arbitrary transient response of the cylinder can be cal-culated from the transfer function by using FFT. For PZT-5 piezoelectric ceramic cylinder,the transfer function,impulse response and step responsehave been calculated.The results show that the impulse response displays a typical minmum phasebehaviour and the cylindrical piezoelectric receiver belongs to the minimum phase system.Therefore,the phase spectrum of transfer function of the receiver can be reconstructed from its amplit     

Wideband Tunable Frequency-Doubling Optoelectronic Oscillator Using a Polarization Modulator and an Optical Bandpass Filter

A wideband tunable frequency-doubling optoeleetronic oscillator(FD-OEO) is proposed and experimentally demonstrated based on a polarization modulator and an optical bandpass filter(OBPF). The central frequency of the correspondingly fundamental OEO could be adjusted by tuning the bandwidth and central frequency of the OBPF, which could also be regarded as a photonic-assisted tunable microwave filter. The frequency tuning range of the FD-OEO covers from 9.5 to 32.8 GHz, and the single sideband phase noise of the fundamental signal is lower than-100 dBc/Hz at an offset of 10 kHz. Moreover, the frequency stability of the generated signal is investigated by measuring its Allan deviation. The Allan deviation of the generated fundamental signal at 10 GHz is 2.39×10~(-9).     

Broadband achromatic phase retarder based on metal-multilayer dielectric grating

A new achromatic phase retarder based on a metal-multilayer dielectric grating structure is designed using the rigorous coupled wave analysis method and the genetic algorithm. The optimized phase retarder can maintain phase retardation around 90°from 900 nm to 1200 nm, and the maximum deviation is less than 4.5% while the diffraction efficiencies of TE and TM waves are both higher than 95%. Numerical analysis shows the designed phase retarder has a high fabrication tolerance of groove depth, duty cycle and incident angle. This achromatic phase retarder is simple in design and stable in performance, and can be widely used in optical systems.     

Phase mismatching analysis of third-harmonic generation in BBO crystal

<正>Phase mismatching for third-harmonic generation(THG) in barium metaborate(BBO) crystal is investigated in detail.Upon using BBO crystal in the TypeⅠ(oo→e) scheme,in the two independent planes (principal section of the crystal and the plane normal to principal section),when the input second-harmonic beam deviates from the expected direction,phase mismatching occurs and the angle deviation produces different effects on the conversion efficiency.We numerically simulate these two cases of phase mismatching and identify the relation between the conversion efficiency and the deviation angle in the air.The computational results indicate that the phase matching tolerance in the principal section is 0.2°(in the air),while the phase matching tolerance in the plane normal to principal section is 4.5°(in the air).After conducting a lab experiment,the results agree perfectly with the computational results,indicating that the deviation angle in the principal section has a greater effect on the conversion efficiency.     

利用小角X射线散射技术研究组分对聚酰亚胺/Al2O3杂化薄膜界面特性与分形特征的影响

采用溶胶-凝胶方法制备无机纳米杂化聚酰亚胺(PI),应用同步辐射小角X射线散射(SAXS)方法研究不同组分杂化PI薄膜的界面特性与分形特征.研究结果表明:散射曲线不遵守Porod定理,形成负偏离,说明薄膜中有机相与Al₂O₃纳米颗粒间存在界面层,界面层厚度在0.54 nm到1.48 nm范围内;随无机纳米组分增加,界面层厚度增加,有机相与无机相作用变强;无机纳米颗粒同时具有质量分形和表面分形特征,其分布、集结是一种非线性动力学过程;随组分增加,其质量分形维数降低 关键词： 小角X射线散射 纳米杂化 聚酰亚胺 界面     

小角X射线散射方法测定二氧化硅干凝胶的平均孔径

提出了当多孔体系的小角X射线散射不遵守Porod定理的情况下,应用Debye法(相关函数法) 和Guinier法(逐级切线法和多级斜线法)计算它们的平均孔径的方法.对不同制备条件下部分 二氧化硅干凝胶的测试,取得了比较一致的结果,并与氮气吸附法测定结果进行了对比. 关键词： 小角X射线散射 二氧化硅干凝胶 平均孔径     

小角x射线散射法研究氧化硅溶胶的制备环境依赖性

根据氧化硅溶胶的不同制备环境(如老化时间、酸碱性和溶剂种类等)，利用小角x射线散射( SAXS)技术，辅以动态光散射等方法，对氧化硅溶胶的界面性质和微结构进行比较性分析.发 现在碱或酸催化下氧化硅溶胶的SAXS结果表现出极大差异，用低分子有机酸作催化剂不仅可 以得到聚硅氧烷大分子，而且有机酸和正硅酸乙酯的酸解反应使溶胶形成内部结构很复杂的 颗粒悬浮体系.溶剂极性越大，则颗粒形貌越不规则.甲酸酸解得到的溶胶颗粒的硅氧四面体 形成程度是所有体系中最差的.发现了在水为溶剂时溶胶SAXS结果中不同寻常的正、负偏离 共存情况，并给出了相应的解释. 关键词： 小角x射线散射 氧化硅 溶胶_凝胶     

Performance on absolute scattering intensity calibration and protein molecular weight determination at BL16B1, a dedicated SAXS beamline at SSRF

The optical system and end‐station of bending‐magnet beamline BL16B1, dedicated to small‐angle X‐ray scattering (SAXS) at the Shanghai Synchrotron Radiation Facility, is described. Constructed in 2009 and upgraded in 2013, this beamline has been open to users since May 2009 and supports methodologies including SAXS, wide‐angle X‐ray scattering (WAXS), simultaneous SAXS/WAXS, grazing‐incidence small‐angle X‐ray scattering (GISAXS) and anomalous small‐angle X‐ray scattering (ASAXS). Considering that an increasing necessity for absolute calibration of SAXS intensity has been recognized in in‐depth investigations, SAXS intensity is re‐stated according to the extent of data processing, and the absolute intensity is suggested to be a unified presentation of SAXS data in this article. Theory with a practical procedure for absolute intensity calibration is established based on BL16B1, using glass carbon and water as primary and secondary standards, respectively. The calibration procedure can be completed in minutes and shows good reliability under different conditions. An empirical line of scale factor estimation is also established for any specific SAXS setup at the beamline. Beamline performance on molecular weight (MW) determination is provided as a straightforward application and verification of the absolute intensity calibration. Results show good accuracy with a deviation of less than 10% compared with the known value, which is also the best attainable accuracy in recent studies using SAXS to measure protein MW. Fast MW measurement following the demonstrated method also enables an instant check or pre‐diagnosis of the SAXS performance to improve the data acquisition.     

Phase transitions in 8CB liquid crystal confined to a controlled-pore glass: Deuteron NMR and small angle X-ray scattering studies

We present results of the deuteron nuclear magnetic resonance (NMR) and small-angle X-ray scattering (SAXS) study of ordering and phase transition behavior of octylcyanobiphenyl (8CB) liquid crystal confined to a controlled-pore glass (CPG) with nontreated and silanes-treated pore surfaces. The deuteron NMR spectra allowed to determine the degree of nematic liquid crystal ordering and also provided an indirect information on the confined 8CB smectic ordering via its influence on the nematic ordering. For the smectic phase these data are supplemented with measurements of the temperature dependence of the first-order SAXS diffraction pattern. The NMR results indicate that the average nematic and smectic order parameters of 8CB in the nontreated CPG are only weakly perturbed by the confinement. The SAXS data further suggest that in confined 8CB for both nontreated and silane-treated CPG a domainlike pattern appears in accordance with the Imry-Ma theorem.     

Phase separation and nanocrystallization in Al92Sm8 metallic glass

Crystallization of Al₉₂Sm₈ metallic glass was investigated in situ using combined small-angle and wide-angle X-ray scattering (SAXS/WAXS) techniques during isothermal annealing at temperatures close to crystallization point. A continuously growing interference maximum shifting progressively towards lower angles was found to develop in SAXS regime. Simultaneously taken WAXS spectra reveal formation of fcc-Al nanocrystalline phase. The analysis of the SAXS/WAXS data indicate that amorphous phase separation is responsible for the nanocrystalline microstructure formation. The primary fcc-Al crystals nucleate inside the Al-rich amorphous regions formed during alloy decomposition and their growth is constrained by the region size.     

Investigation of the Melt‐Crystallization of Polypropylene by a Temperature Slope Method

Abstract

To investigate the in‐situ ordering process of isotactic polypropylene (iPP) from a melt state, a stationary growth front was prepared by the temperature slope crystallization (TSC) method. During the melt‐crystallization, iPP was crystallized into the α‐phase or β‐phase depending on the crystallizing conditions. The mechanism of the melt‐crystallization at the growth front was precisely observed by wide‐angle and small‐angle x‐ray scattering (WAXS and SAXS) using a strong synchrotron beam. In the TSC apparatus, the sample was crystallized in between a heater, controlled to 220°C, and a cooler, cooled by water to 25°C. We define the z‐axis parallel to the temperature gradient. A‐lamellae and B‐lamellae are also defined as those whose lamellar normal are perpendicular and parallel to the z‐axis, respectively. In a sample‐stop (SS) stage before the TSC, the original α‐phase lamellae became thicker, approaching to the melt‐solid boundary by annealing. The annealing process showed that the α‐phase B‐lamellae remained and the SAXS reflection was stronger on the meridian near the melt‐solid boundary in the SS stage. In the beginning of the TSC, the α‐phase B‐lamellae developed as a primary crystallization. During secondary crystallization under high supercooling, the SAXS cross pattern appeared showing that the α‐phase developed both A‐ and B‐lamellae. As the growth direction of A‐lamellae is parallel to the z‐axis, A‐lamellae grow faster than B‐lamellae. By the self‐epitaxial mechanism on the side surface of the A‐lamellae, the B‐lamellae grow on the base of the A‐lamellae. Following appearance of a spontaneous β‐nucleus, the β‐phase lamellae grew preferentially, excluding the α‐phase, and occupied the whole area of the sample. In this case also, A‐lamellae are advantageous to grow because of the growth direction parallel to the z‐axis. As a result, the SAXS β‐phase reflection appeared on the equator.     

Investigation of surface heterogeneity in thermally treated controlled porous glasses and systems silica gels/borate crystals by means of the SAXS method

Heating of controlled porous glass (CPG) in the temperature range 400–700°C leads not only to a dehydroxylation process of the surface but also brings about a diffusion of the boron atoms remaining in the silica network of CPG towards the glass surface. Some authors assume that a along thermal exposure can cause the formation of B₂O₃ crystals in the pores. In this paper the CPGs possessing different mean pore diameters before and after their thermal treatment were investigated by the SAXS (small angle X-ray scattering) method. The SAXS method is very useful in such cases because there are two sources of X-ray scattering: pores in glass and crystallites of the borate phase. The presence of these two sources is responsible for the change of the intensity of small angle X-ray scattering in comparison to X-ray scattering of the initial porous glass (without borate crystallites). In consequence, the pore size distribution function, calculated from the SAXS data, does not agree with the analogous one calculated from mercury porosimetric data. For the confirmation of the above artificial systems composed of silica gle with either deposited H₃BO₃ or Na₂B₄O₇ were investigated. It appears from the presented data that there is a possibility to investigate the kinetics of the crystallization process of borate crystallites by means of the SAXS method. SAXS also allows one to control the process of the removal of the borate phase from the pores of CPG. It can be concluded from the obtained results that long time thermal heating causes the formation of borate crystallites in pores of CPG and that these crystallites are xNa₂O·yB₂O₃ (where y ? x) rather than B₂O₃.     

TIME-RESOLVED SAXS/WAXS STUDY OF PHASE BEHAVIOR AND CRYSTALLIZATION IN POLYMER BLENDS

Real-time SAXS and WAXS patterns have been simultaneously obtained during isothermal melt-crystallization of blends of low-molecular-weight poly(ethylene oxide) (PEO) and poly(methyl methacrylate) (PMMA). The analysis of results shows that the originally homogeneous, single-phase polymer blend separates into two phases. The PMMA molecules diffuse from the blend and form completely segregated regions while PEO starts to crystallize. The first and dominating effect at the beginning of crystallization is the formation of unstable lamellae of nonintegrally folded chains (NIF). The real-time crystallinity and density of the PEO crystalline phase in absolute units were obtained from the time-resolved SAXS/WAXS results. The structure development proceeds in two steps. A very fast evolution of PEO crystals from the melt starts to crystallize in disordered NIF lamellae with thick amorphous interlayers and with a lower density of crystalline phase. The steep growth of crystallinity and crystalline density mean quick thickening of crystalline part of lamellae and improvement of their crystalline structure. In the second step, the structure of the crystalline phase gradually improves and crystallinity grows very slowly. The recrystallization of NIF lamellae into extended chain lamellae (EC) and lamellae with once folded chains (1F) proceeds during both stages of crystallization.