“FLIPSY”—A New Solvent-Suppression Sequence for Nonexchanging Solutes Offering Improved Integral Accuracy Relative to 1D NOESY

A new method of solvent suppression is described, based on presaturation in combination with volume selection; the name “FLIPSY” is proposed for this sequence. A low-flip-angle pulse is used for excitation, immediately followed by two 180° pulses, each of which is independently phase cycled through Exorcycle. The phase-cycled inversion pulses achieve volume selection in a way similar to the widely used 1D NOESY sequence, thereby largely eliminating any residual “hump” signal from the solvent. The two 180° pulses combine to produce a net 360° rotation forzmagnetization and either a 180° or a 360° rotation for transverse magnetization, depending on the step in the phase cycle. This allows the overall flip angle of the sequence to be controlled by adjusting the length of the initial excitation pulse. It is demonstrated that this property allows one to choose freely a suitable compromise between signal strength and integral accuracy when using FLIPSY, just as when using single-pulse excitation. Such a choice cannot be made when using 1D NOESY, since the effective flip angle in that experiment is always 90°. The application of FLIPSY to recording LC-NMR spectra is demonstrated.     

Highly sensitive interferometric testing of deviation of the wedge angle of transparent plates

To improve the accuracy of the interferometric method of testing the wedge angle of a transparent plate, we propose using nonlinear recording of holograms of the reference and tested plates on different carriers and creating interference patterns that map the deviation of the angle, using higher orders of light diffraction on the holograms, with improved sensitivity. The increasing accuracy of the interferometric method of testing is provided by waves diffracted on holograms of the reference and tested plates in higher diffraction orders. Results of experimental testing of the method are presented.     

微楔形镜加工技术研究

微楔形镜的加工不能像平行平面元件那样,采用大块抛光,切片分割的办法。针对零件尺寸小、精度要求高的特点,研究了加工过程中的粘结上盘、面形精度控制和楔形角检测等技术,设计了吸附式粘结上盘和楔形角测量等专用装置,应用于尺寸为3×3×1mm(6°)的Nd∶YVO4(掺钕钒酸钇)晶体批量生产中,提高了零件的面形精度和加工可靠性。测试结果表明:面形精度优于λ/10(λ=632.8nm),表面光洁度达0/0级,楔形角合格率达98%以上。     

在反转恢复测试中磁化矢量的演化特征:辐射阻尼效应

在强辐射阻尼存在下,水样(90% H₂O in D₂O)的反转恢复实验表明:当两脉冲的相位相差180°且反转脉冲角<180°时,或两脉冲相位一致但反转脉冲角>180°时,在检测期观测到的信号强度将不发生从负极大值到正极大值的突变;在同样的条件下,如果存在频率偏置,信号强度存在波动,即beating效应.只有当两脉冲的相位一致而反转脉冲角<180°时,或两脉冲的相位相差180°但反转脉冲角>180°时,在检测期信号强度才发生突变,即jumping效应.这些现象都可通过辐射阻尼理论予以合理地解释.另外,在检测期当磁化矢量运动到-z轴附近(对应于τ=T_rdln{tan[(π±δ)/2]}),信号强度与理论预计的偏差实际上与T₁弛豫效应有关.     

An improved reflectometric method to measure the azimuthal anchoring energy of nematic liquid crystals

Some years ago we developed an automatized reflectometric method to measure the surface azimuthal anchoring energy of nematic liquid crystals on an optically isotropic substrate. This method provides a high accuracy and sensitivity but requires the use of wedge glass plates and a sufficiently high anisotropy of the intensity reflectivity coefficients. This latter condition restricts greatly the number of possible substrates that can be investigated with this technique. Here we develop a new reflectometric method which offers comparable or better accuracy and sensitivity but does not require wedge plates and high anisotropy of the reflectivity coefficients. The method is fully automated and provides a direct measurement of the azimuthal director angle. The experimental procedure exploits the dependence of the reflectivity tensor on the surface director orientation. The measurement of the azimuthal angle does not require any knowledge of the optical parameters of the nematic material and of the optically isotropic substrate, and provides an absolute accuracy better than 0.2^° in the whole range 0-360^° and a sensitivity better than 0.1^°. This reflectometric method can be also used with weakly anisotropic substrates as well as thin rubbed polymeric layers. In this latter case, the effective uncertainty in the measurement of the director azimuthal angle depends on the substrate anisotropy. A simple and direct experimental procedure to estimate this uncertainty is proposed. Received 8 January 2002 and Received in final form 27 February 2003 / Published online: 15 April 2003 RID="a" ID="a"e-mail: faetti@df.unipi.it     

A self-method for resolving the problem of apparent LWIR emissivity for quantitative thermography up to 130 °C

In a previous work, we succeeded in connecting normal LWIR apparent emissivity to the spectral one of an aluminum nitride ceramic plate. The key problem was the knowledge of the effective spectral bandwidth in use in the system. Hence we have developed an analyzer which permits to identify the spectral bandwidth of IR system using only its raw data. It proceeds by minimizing the dispersion from linearity of the characteristic thermosignals/integrated radiance over a temperature range of the IR system. The capacities of the analyzer are tested for five commercial cameras. Each of these systems exhibits a similar formatting process implemented during the thermogram recording. The effective spectral bandwidth shows plausible values. It varies significantly from one model to the other and the residual non-linearity is connected to the NETD of the IR system. The robustness of the apparent emissivity measurements is also tested with the aid of emissivity reference of 0.5. The overall accuracy of the method is less than 1%, depending on the specular or diffuse part of the reflected irradiation. Applied in field situation, the method is suitable to detect absolute variation of emissivity of less than 6 ⋅ 10⁻³. We use the analyzer to determine the spectral bandwidth of a commercial 320 × 240 microbolometer uncooled IRFPA camera which had already served to characterize the normal LWIR apparent emissivity of the aluminum nitride ceramic plate. By using the spectral response of the two major microbolometer sensor technologies, the general formulation of apparent emissivity matches our apparent emissivity measurements. An agreement better than 0.6% in absolute value and a less than 6 ⋅ 10⁻³%/°C dispersion are found over the entire temperature range [40–130 °C].     

Reduction of the error in measuring the wedge angle of transparent plates in holographic reverse-shearing interferometry

To reduce the error in measuring small wedge angles of transparent plates by holographic reverse-shearing interferometry, it is proposed to form a pair of interference patterns using joint plate rotation and alternate tuning to an infinitely wide band in the right and left patterns. The results of experimental approval of the method used to form interferograms of a glass plate with a small wedge angle, which indicate a higher sensitivity of this method and, as a consequence, a smaller measurement error, are presented.     

缺陷态对4340钢-环氧树脂二维声子晶体带隙的影响

采用平面波展开法及平面波超元胞法研究缺陷态对4340钢-环氧树脂二维声子晶体带隙的影响. 以环氧树脂作为基底,把正方形结构排列的4340钢均匀的插入基底中,计算完整晶体、45°线缺陷态晶体、90°线缺陷态晶体、135°线缺陷态晶体、180°线缺陷态晶体的带隙. 结果表明,缺陷态的带隙宽度与完整晶体的带隙宽度相比最大可增大约31倍;对于不同的缺陷结构在F=0.1-0.9的范围内均有带隙出现且随着缺陷态角度的增大. 同时讨论带隙数目N,最低带隙相对宽度Δω/ω_g与填充率F之间的关系. 关键词： 缺陷态 带隙宽度 带隙数目     

强梯度复杂流场中的粒子动力学响应试验研究

示踪粒子在(高)超声速流场中的动力学响应是粒子成像测速等粒子示踪测量技术的关键问题之一.现有文献对粒子动力学响应的试验测量往往是通过单个斜激波响应的测量方法.然而,当示踪粒子用于测量高速飞行器发动机内部复杂的激波串流场时,粒子将经历由多道激波导致的速度、压力、黏性等剧烈变化.本文结合目前(高)超声速飞行器的研究热潮,重点关注示踪粒子在应用于发动机内部具有连续激波的复杂流场测量中存在的跟随性评估方面,开展了一系列的相关试验研究.包括测量超声速风洞的喷管出口速度分布以验证测试系统的性能,在马赫4.2和3.0流场中测量了粒子对二维10°和15°单斜劈绕流中的斜激波动力响应,并测量了模拟发动机内部连续梯度的双斜劈粒子斜激波动力响应.结合粒子动力学的理论模型,得到了各状态的粒子弛豫时间、弛豫距离、Stokes数.基于图像方法、统计学规律分析了激波非定常抖动对测量结果的影响,并对测量结果进行了修正.结果显示,相同斜劈角度下,马赫数越高,粒子的弛豫时间、弛豫距离就越大.但是在相同的来流马赫数下,斜劈角度越大,粒子的弛豫时间、弛豫距离反而减小.在强梯度之后由于流场的雷诺数和黏性系数变化剧烈,粒子的跟随性降低了大约5.7%,stokes数增加了约1%.虽然在本文条件下Stokes数仍满足超声速流场对粒子跟随性的要求,但粒子响应的降低无疑是值得关注的,尤其是当其被应用于具有更多连续梯度的复杂流场测量中.     

Influence of defect states on band gaps in the two-dimensional phononic crystal of 4340 steel in an epoxy

The band structures of a new two-dimensional triangle-shaped array geometry of 4340 steel cylinders of square cross section into epoxy resin were studied by the plane-wave expansion and supercell calculation method. The band gaps of this type of phononic crystals with different defects were calculated such as defect-free, 60° crystal linear defect states, 120° crystal linear defect states, and 180° crystal linear defect states. It was found that the band gap will emerge in different linear defects of the phononic crystals and the bandwidth of linear defect states is larger than that of the free-defect crystal by about 2.14 times within the filling fraction F=0.1-0.85. In addition, the influence of filling fraction on the relative width of the minimum band gap is discussed.     

Determining the phase of line objects by measuring their intensity in dark field and bright field illumination

The in situ phase of a transparent line object can be calculated from measurements of its bright field and dark field intensity. If the sampling aperture is a slit, the background can be subtracted out for increased accuracy. This method can measure phase over a range of approximately 3° to 180°. The theory has been verified by means of an indirect experiment.     

Simple synthesis of ironIII sulfophenyl phosphate nanosheets as a high temperature inorganic–organic proton conductor

Iron^III sulfophenyl phosphate (FeSPP) is successfully synthesized by an optimized process from the reaction of iron^III chloride and m-sulfophenyl phosphonic acid (msPPA) by a simple and environmentally friendly method. Experimental results show FeSPP has a kind of layered structure, and multilayer sheet is about 2 nm thick. FeSPP exhibits good thermal stability and does not decompose under 200 °C. Protons transfer through vehicle and Grotthuss mechanisms at different relative humidities (RH). The conductivity of FeSPP can reach to 0.115 S/cm at 180 °C and RH?=?100 %. Under this condition, vehicle mechanism plays the leading role, and the Grotthuss mechanism plays the minor role. At low RH, Grotthuss plays the leading role, and vehicle plays the minor role. In a drying oven at 180 °C, the proton conductivity remains 2.15?×?10^?3 S/cm. Good conductivities at different RH and thermal stabilities clearly demonstrate that FeSPP is a highly effective conductor. It can be used as catalysts, chemical sensors, and in the preparation of composite membrane.     

一种新型慢波结构TM01-TE11模式转换器的数值模拟

 设计了一种新型L波段慢波结构式圆波导TM₀₁-TE₁₁模式转换器，该转换器的尺寸为φ15.0 cm×40.8 cm，通过金属分割片将圆波导分成两个180°区域并在其中一个区域内设置半环形慢波结构。当TM01入射时，在两个区域内激励起扇形波导TE11模式，由于慢波结构的存在，该模式在两个区域内的传播常数不一样。适当调节慢波结构的参数，可使两个区域内传输的扇形TE11模式在金属分割片尾部相位相差180°，这两个扇形TE11模式耦合成为圆波导TE11模式输出，实现模式转换。建立数值模型并进行了模拟，结果表明在工作频率1.8 GHz处转换效率96%，反射率低于0.04，功率容量超过1.7 GW。     

Determination of the Disperse Composition of a PbO Suspension Containing Aggregates of Particles of Lamellar Shape by the Laser-Polarimetry Method

The results of measurements of the scattering matrix at a wavelength of 0.63 μm in the range of scattering angles of 10°–155° are presented for an aqueous suspension of lead oxide containing particles of plate form and their aggregates of monomers with dimensions of ~5 nm. The results of the measurements are compared with the results of calculations for axially symmetric scatterers (ellipsoids of rotation, cylinders). It is shown that the presence of aggregates affects the scattering properties of such a medium. The results of reconstructing the distribution of particles of a disperse medium in sizes from the measurements data of the scattering matrix are presented. The reconstruction of the distributions was carried out by solving the problem of optimizing the sum of the squared deviations of the experimental and calculated values of matrix elements in the framework of the model of axially symmetric scatterers. It is shown that the distribution of particles by sizes is more accurately reconstructed by minimizing the sum of the squares of the deviations for the sum of the diagonal elements. The obtained distribution is compared with the distribution measured by the method of dynamic light scattering.     

Design of a wedge plate for polarization-preserving angular shifter

It is shown that by using a wedge plate, the incident direction of light propagation can be rotated as necessary while still preserving beam polarization. The basic conditions of these preservations of polarization are deduced. For numerical demonstration, it is shown that a collimated beam with +45° linear polarization can be guided to any pre-settled direction where the square of ellipse ratio variation in the polarization is less than 0.0001%, while the variation of squared ellipse ratio of a right circular polarization beam is kept under 0.1%.     

Pressure dependence of the ionic conductivity of Na- and Na–Rb borate glasses

The ionic conductivity of Na- and Na–Rb borate glasses is investigated as a function of hydrostatic pressure. Activation volumes of the dc conductivity are obtained from pressure-dependent ac conductivity measurements at a constant temperature of 180 °C. The activation volume of Na borate glasses decreases with increasing alkali content. It depends linearly on a separation parameter which is defined as the ratio of the average ionic distance and the average network atom distance. The activation volume of Na–Rb borate glasses increases from both end-members towards the mixed-alkali regime and passes through a maximum near the relative content Na/(Na + Rb) = 0.4. In addition to mobility anomalies, observed earlier in these borate glasses, the maximum in the activation volume is a further important fingerprint of the mixed-alkali effect.     

Wedge plate interferometry: a new dual field configuration for collimation testing

A method of deriving a dual field fringe pattern from a single wedge plate for collimation testing is presented. The proposed technique uses a wedge plate and a 90° prism retroreflector to form two interference fields. With the two sets of fringes, the technique provides twofold increase in sensitivity and has its own reference.     

Numerical study of the extinction matrix for a plate crystal

Energy and polarization characteristics of optical radiation passed through a semitransparent plate crystal with a preset orientation in space are studied numerically within the framework of the method of physical optics. Results of calculations of the extinction matrix elements versus particle size, refractive index, crystal orientation, and incident radiation wavelength (from 0.5 to 15 μm) are presented. It is demonstrated that K₁₁, K₁₂, and K₃₄ are most informative among the elements of the extinction matrix. It is established that the first of them is most sensitive to changes in the microphysical and orientational parameters of the particle when the angle of radiation incidence on the plate changes from 0 to 20°, and the nondiagonal elements are most sensitive when the angle of radiation incidence is greater than 40°. The characteristics of the total field scattered near the forward direction are determined. It is established that their dependence on the physical parameters of the crystal is most strong at scattering angles smaller than or equal to 4° and wavelengths from the IR range (in particular, from the atmospheric transparency window).     

A Fourier transform speckle method to determine the change in angle of illumination

It is analytically shown that the position of the Fourier transform of the speckle pattern produced by a coherently illuminated, diffusely reflecting surface depends upon its angle of illumination. A method is proposed to measure small changes in this angle by doubly exposing the photographic plate with the original and laterally displaced Fourier transforms of the object speckle. The method is well suited for accurate measurements of the wedge angle and tilt of optical surfaces and to determine variations in refractive index or temperature of axially symmetric phase objects.     

Interferometric determination of the high-intensity laser-pulse-material interaction site

We developed a method that accurately determines an unknown position of the high-intensity laser-pulse-material interaction site on the front side of a plate. It is based on interferometric measurements of a normal displacement at known positions on the plate’s rear side. The displacement is caused by reflections of various pulsed-laser-induced mechanical waves. We have superseded the long-established time-of-flight approach with the improved, triple-echo method. To accurately locate the origin of the laser-induced ultrasound on the plate with a known thickness, we only need to detect the arrivals of the first three consecutive mode unconverted waves. Our method works without knowing the propagation velocities of various ultrasonic waves and additionally solves some time-related drawbacks of the conventional time-of-flight approach. The relative uncertainty of the measured source-receiver separations obtained with the presented method is less than 0.01.