Synthesis,characterization, and curing kinetics of novel ladder‐like polysilsesquioxanes containing side‐chain maleimide groups

Two ladder‐like polysilsesquioxanes (LPS) containing side‐chain maleimide groups have been synthesized successfully by reacting N‐(4‐hydroxyphenyl)maleimide (HPM) with LPS containing 100 mol % of chloropropyl groups (Ladder A ) and 50 mol % of each methyl and chloropropyl group (Ladder B ). HPM was synthesized by reacting maleic anhydride with 4‐aminophenol, and the resulting amic acid was imidized using p‐toluenesulfonic acid as a catalyst (Scheme 1 ). The LPSs were characterized by Fourier transform infrared (FTIR), ¹H nuclear magnetic resonance (NMR), proton‐decoupled ¹³C NMR, ²⁹Si NMR, wide‐angle X‐ray diffraction (WAXD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Characterization indicated that these polymers had ordered ladder‐like structures with possible defects. These polymers were soluble in common solvents at ambient temperature, which suggested that they were not crosslinked. Both the polymers and the HPM were cured, and their kinetics were followed by dynamic DSC. The Ozawa and Kissinger methods were used to calculate activation energies for curing. Curing increased the temperature at which both 5% weight loss and maximum rate of weight loss were observed. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 4036–4046, 2004     

Surface roughness investigation of semi-conductor wafers

Conventionally, surface roughness is predominantly determined through the use of stylus instruments. However, there are certain limitations involved in the method, particularly when a test specimen, such as a silicon wafer, has a smooth mirror-like surface. Hence, it is necessary to explore alternative non-contact techniques. Light scattering has recently been gaining popularity as an optical technique to provide prompt and precise inspection of surface roughness. In this paper, the total integrated scattering (TIS) model is modified to retrieve parameters on surface micro-topography through light scattering. The applicability of the proposed modified TIS model is studied and compared with an atomic force microscope. Experimental results obtained show that the proposed technique is highly accurate for measuring surface roughness in the nanometer range.     

A study of electrostatic spring softening for dual-axis micromirror

Electrostatic spring softening is an important characteristic of electrostatically actuated dual-axis micromirror, since it lowers the resonant frequencies. This paper presents an approach based on approximating the electrostatic forces by the first-order Taylor's series expansion to investigate this characteristic. The dual-axis micromirror studied in this paper has three motion modes, two torsional (about x- and y-axis, respectively) and one translational (about z-axis). The stiffnesses of all these modes are softened by a DC bias voltage applied to the mirror plate. The resonant frequencies are lowered with the increment of the bias voltage. The relationship of the bias voltage and the resonant frequencies of all the motion modes is derived. The analytical results show that the resonant frequency curves are affected by the capacitor geometries, i.e. the gap between the mirror plate and the electrodes and the electrodes size. The lowering curves drop slowly when the bias voltage is small. While for large bias voltage, the lowering curves drop rapidly. The experiment results are consistent with those obtained by the analytical approach.     

Structure and properties of (1−x)(0.6Pb(Zn1/3Nb2/3)O3-0.4Pb (Mg1/3Nb2/3)O3)-xPbTiO3 thin films with perovskite phase promoted by polyethylene glycol

The preferential formation of a pyrochlore structure is a knotty problem in the preparation of Pb(Zn_1/3Nb_2/3)O₃ (PZN)-based thin film materials and its presence is significantly detrimental to the dielectric and piezoelectric properties. In this study, 40 mol% of PZN was replaced with Pb(Mg_1/3Nb_2/3)O₃ (PMN) for obtaining a perovskite composition around a morphotropic phase boundary (MPB), (1−x)(0.6PZN-0.4PMN)-xPT ((1−x)PZMN-xPT, PT: PbTiO₃) where x = 0.23. The thin films with this composition were prepared with a polyethylene glycol (PEG) modi-fied sol-gel method on LaAlO₃ substrates. The microstructural evolution of the films on heat treatment was examined with X-ray diffraction. With the aid of PEG, the formation of the pyrochlore phase was suppressed and the perovskite phase formed directly from the amorphous gel film. The multilayer films with a thickness around 0.25 μm showed a single perovskite phase without any detectable pyrochlore structure. Microscopic images showed uniform grain size of a few tens of nanometers. The role of the polymer dramatically promoting the perovskite phase was investigated with the aid of X-ray photoelectron spectroscopy and thermal analysis. The dielectric constant of the obtained film was 4160 at 1 kHz. The film demonstrated typical ferroelectric hysteresis loops and exhibited excellent piezoelectric performance.     

Bacteria and cancer cell pearl chain under dielectrophoresis

In this work, we aim to observe and study the physics of bacteria and cancer cells pearl chain formation under dielectrophoresis (DEP). Experimentally, we visualized the formation of Bacillus subtilis bacterial pearl chain and human breast cancer cell (MCF-7) chain under positive and negative dielectrophoretic force, respectively. Through a simple simulation with creeping flow, AC/DC electric fields, and particle tracing modules in COMSOL, we examined the mechanism by which bacteria self-organize into a pearl chain across the gap between two electrodes via DEP. Our simulation results reveal that the region of greatest positive DEP force shifts from the electrode edge to the leading edge of the pearl chain, thus guiding the trajectories of free-flowing particles toward the leading edge via positive DEP. Our findings additionally highlight the mechanism why the free-flowing particles are more likely to join the existing pearl chain rather than starting a new pearl chain. This phenomenon is primarily due to the increase in magnitude of electric field gradient, and hence DEP force exerted, with the shortening gap between the pearl chain leading edge and the adjacent electrode. The findings shed light on the observed behavior of preferential pearl chain formation across electrode gaps.     

Surface profile measurement of low-frequency vibrating objects using temporal analysis of fringe pattern

A simple and accurate algorithm (phase scanning method) is proposed for 3D surface contouring and dynamic response determination of a vibrating object. A sinusoidal fringe pattern is projected onto a low-frequency vibrating object by a programmable liquid crystal display projector. The fringe patterns are captured by a high-speed CCD camera with a telecentric gauging lens. Phase values are evaluated point by point using phase scanning method. From the phase values of each point on the object, the contour of the specimen at different instants of vibration can be retrieved. In this paper, a small vibrating coin is used to demonstrate the validity of the method and the experimental results are compared with test results on a stationary coin using four-step phase shifting and fast Fourier transform methods. The technique is especially useful in applications where the vibrating object has a complicated shape.     

Fringe contrast-based 3D profilometry using fringe projection

Quality-guided algorithm is a widely used method in phase unwrapping. This paper shows an accurate quality map based on fringe contrast for 3D shape measurement. Phase-shifted fringe patterns are projected onto an object surface by a programmable liquid crystal projector and recorded by a CCD camera. A wrapped phase map and a fringe contrast map are extracted from the deformed fringe patterns by the phase-shifting technique. Guided by the contrast map, the quality-guided unwrapping algorithm minimizes unwanted shadow and non-uniform surface reflectance effects and is able to retrieve a correct surface profile. Validity of the proposed method is tested on a fish model and a cutting tool specimen.     

Creep deformation measurement using quartz optical fiber

This paper describes an optical system for high temperature creep strain measurement using quartz optical fiber, super long working distance microscope and digital image processing techniques. In this system one end of the quartz optical fibers is arrayed in a small area on the specimen surface and the other end is illuminated by a laser beam. The fiber ends on the specimen surface form the spot array. The small optical spots on the specimen are tracked by a CCD camera and the images are processed by digital image processing software. The diameter of each quartz fiber is 100 μm and the fibers can be arrayed in a small area. The local strains are determined by measuring the variety of relative distance between two spots. Experimental results of local creep strain on the welding joints of 15CrMo and HK40 at 850°C are obtained.     

Regiospecific Formation and Unusual Optical Properties of 2,5‐Bis(arylethynyl)rhodacyclopentadienes: A New Class of Luminescent Organometallics

A series of 2,5‐bis(arylethynyl)rhodacyclopentadienes has been prepared by a rare example of regiospecific reductive coupling of 1,4‐(p‐R‐phenyl)‐1,3‐butadiynes (R?H, Me, OMe, SMe, NMe₂, CF₃, CO₂Me, CN, NO₂, ?C?C‐(p‐C₆H₄?NHex₂), ?C?C?(p‐C₆H₄?CO₂Oct)) at [RhX(PMe₃)₄] ( 1 ) (X=?C?C?SiMe₃ ( a ), ?C?C‐(p‐C₆H₄?NMe₂) ( b ), ?C?C?C?C?(p‐C₆H₄?NPh₂) ( c ) or ?C?C?{p‐C₆H₄‐C?C?(p‐C₆H₄‐N(C₆H₁₃)₂)} ( d ) or Me ( e )), giving the 2,5‐bis(arylethynyl) isomer exclusively. The rhodacyclopentadienes bearing a methyl ligand in the equatorial plane (compound 1 e ) have been converted into their chloro analogues by reaction with HCl etherate. The rhodacycles thus obtained are stable to air and moisture in the solid state and the acceptor‐substituted compounds are even stable to air and moisture in solution. The photophysical properties of the rhodacyclopentadienes are highly unusual in that they exhibit, exclusively, fluorescence between 500–800 nm from the S₁ state, with quantum yields of Φ=0.01–0.18 and short lifetimes (τ=0.45–8.20 ns). The triplet state formation (Φ_ISC=0.57 for 2 a ) is exceptionally slow, occurring on the nanosecond timescale. This is unexpected, because the Rh atom should normally facilitate intersystem crossing within femto‐ to picoseconds, leading to phosphorescence from the T₁ state. This work therefore highlights that in some transition‐metal complexes, the heavy atom can play a more subtle role in controlling the photophysical behavior than is commonly appreciated.