Estimating crystallinity in high density polyethylene fibers using online Raman spectroscopy

Online Raman spectra, obtained at different points along the spin line during pilot‐scale nonisothermal melt spinning of high density polyethylene (HDPE) fibers, are presented for the first time. The fraction of the crystalline phase corresponding to each spectrum was determined from the normalized integrated intensity of the 1418 cm^?1 Raman band. It is well established that this band represents the orthorhombic crystalline phase in polyethylene. The estimates of percent crystallinity obtained from decomposition of the Raman spectrum were compared with the percent crystallinity from differential scanning calorimetry (DSC) measurements. It is concluded that online Raman spectroscopy can be successfully used to monitor the development of crystallinity in HDPE fibers as a function of distance from the spinneret. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 545–549, 2003     

X-ray diffraction and Raman scattering in SbSI nanocrystals

Lattice structure and rod-like shaped SbSI nanocrystals obtained by ball milling with rod thickness down to 70 nm, as estimated from X-ray diffraction (XRD) and electron microscopy, is similar to that of the bulk crystals. The dependence of the grain size on the milling duration is discussed in view of the chain-like crystalline structure of SbSI. Possible factors, responsible for the observed Raman line broadening, are discussed, scattering by surface phonons being considered the predominant one.     

流量比对等离子体基团分布和薄膜结构的影响

使用光强标定的发射光谱(AOES)测量了CHF3／C6H6混合气体的微波电子回旋共振(ECR)放电等离子体中基团的分布状态。实验发现随着CHF3流量的增加，成膜基团CF、CF2、CH等的相对密度增大，而刻蚀基团F的密度也会增加，从而使得a—C：F薄膜的沉积速率降低。同时红外吸收谱(IR)分析表明，在高CHF3流量下沉积的a—C：F薄膜中含有更高的C—F键成分。可见在a—C：F薄膜的制备中CHF3／(CHF3 C6H6)流量比是重要的控制参量。     

Cs-K混合蒸气中Cs(8D)+K(4S)碰撞能量转移

在Cs-K混合蒸气中，两步激发Cs原子到8D态，观察了Cs(8D) K(4S)→Cs(5D) K(4P)碰撞能量合并逆过程(REP，reverse energy pooling)。应用双调制技术探测K(4P)原子发射的荧光，基态K原子密度用光学吸收方法测量。得到了REP速率系数，讨论了其它过程对速率系数的影响．     

Synthesis and luminescence of Sr2CeO4 fine particles

Fine particles of a blue emission phosphor Sr₂CeO₄ have been synthesized using a chemical co-precipitation technique, and the textual and luminescent properties were compared with the one synthesized by the conventional solid-state reaction method. Particle size and distribution of the Sr₂CeO₄ fine powder prepared by the co-precipitation process were smaller and narrower than those obtained by the samples prepared from the conventional one. The emission intensity of the fine particles was equal to that of the larger particles prepared from the solid-state reaction, on the contrary to the general tendency that emission intensity decrease with particle size reduction. Although no Ce³⁺ peaks were observed in EPR measurements, X-ray photoelectron spectra of the samples clearly elucidated the existence of Ce³⁺ only on the surface of Sr₂CeO₄.     

Reduction mechanism of tioglycolic acid on keratin fibers using microspectrophotometry and FT-Raman spectroscopy

In order to investigate the reduction mechanism of thioglycolic acid (TG) on the keratin fibers, cross-sectional samples of white human hair treated with TG were prepared. The heterogeneous reaction between TG and keratin fibers involving the diffusion of TG into human hair was analyzed at the molecular level using microspectrophotometry and FT-Raman spectroscopy. The diffusion of TG into human hair clearly increased by increasing the treatment time and by raising pH. The TG relative concentration and the disconnected relative concentration of disulfide (–SS–) groups at various depths of the hair samples with pH 9.0 were in good agreement, indicating that the reaction rate (the disconnection of –SS– groups) was faster than the diffusion rate of TG into human hair. From these experiments, we demonstrated that TG diffuses gradually beyond the cuticle region, and toward the inside of the cortex region along with the disconnection of –SS– groups.     

Time-resolved spectroscopy of infrared active vibrations in 2,5-dioctyloxy poly(phenylene vinylene) films

We report on picosecond time resolved spectroscopy of photogenerated infrared active vibrations in thin films of 2,5-dioctyloxy poly(phenylene vinylene). We excited the films by ?4 ps long pulses of 565 nm laser light with 2×10¹³ photons/cm² per pulse and repetition rate of 76 MHz. We then followed the temporal evolution of the infrared active vibrational (IRAV) spectrum using a subsequent, variably delayed, weak tunable IR probe pulses of similar temporal duration. Under these conditions, we show clear spectroscopic evidence for photogenerated infrared active vibrations at times which are shorter than our temporal resolution (<4 ps). We suggest that the transient IRAV absorption is due to secondary polarons formation following exciton dissociation.     

古陶片年龄与烧结温度测定中的计算机模拟

介绍用已知年龄和烧结温度的古陶片穆斯堡尔超精细参数与年龄和烧结温度的实验关系曲线作基础，应用计算机模拟程序，自动求出未知陶片的年龄和最高烧结温度的方法。     

Preparation, Characterisation and Catalytic Behaviour of a New TeVMoO Crystalline Phase

TeM_xMo_1.7O mixed oxides (M = V and/or Nb; x = 0-1.7) have been prepared by calcination of the corresponding salts at 600 °C in an atmosphere of N₂. A new crystalline phase, with a Te/V/Mo atomic ratio of 1/0.2-1.5/1.7, has been isolated and characterised by XRD and IR spectroscopy. This phase is observed in the TeVMo or TeVNbMo mixed oxide but not in the TeNbMo mixed oxide. The new crystalline phase shows an XRD pattern similar to Sb₄Mo₁₀O₃₁ and probably corresponds to the M1 phase recently proposed by Aouine et al. (Chem. Commun. 1180, 2001) to be present in the active and selective MoVTeNbO catalysts. Although these catalysts present a very low activity in the propane oxidation, they are active and selective in the oxidation of propene to acrolein and/or acrylic acid. However, the product distribution depends on the catalyst composition. Acrolein or acrylic acid can be selectively obtained from propene on Nb-free or Nb-containing TeVMo catalysts, respectively. The presence of both V and Nb, in addition to Mo and Te, appears to be important in the formation of acrylic acid from propene.     

EIS evaluation of the filiform corrosion of aluminium coated by a cataphoretic paint

Filiform corrosion is mainly considered as a cosmetic attack and is undesirable in most applications. The initiation and propagation of the filaments are related to different parameters such as the presence of defects, the permeability of the coating to water and oxygen, the adherence of the paint system and the presence of salts.

The aim of this work is to study the behaviour of painted aluminium samples towards filiform corrosion or delamination. The 6082 Aluminium alloy was selected and the samples were covered with a cataphoretic epoxy primer without lead (PPG Industries France). Prior to the application of the electrocoat, the samples were pre-treated by a commercial Zr/Ti or chromate conversion treatment or simply etched with a commercial acid etching product.

Filiform corrosion was studied by the normalized test (ISO/DIS 4623): painted and scratched samples were inoculated in HCl and exposed in a constant humidity chamber at 40 °C and 82% RH for 3 weeks. After exposure the samples were subjected to a visual and optical microscopic examination.

Electrochemical impedance spectroscopy was used to study the sensitivity to filiform corrosion. The operating mode of this test is similar to the normalized one. The samples were scratched before inoculation for 1 h in HCl and then exposed to the humidity chamber for a maximum of 4 days. The samples were tested by EIS in an acidified 0.1 M Na₂SO₄ electrolyte solution. The resulting impedance spectra were analyzed with an appropriate equivalent electrical circuit which allows the evaluation of the exposed metallic surface area, directly related to the extent of filiform corrosion or delamination. Different parameters were varied: the exposure time in the humidity chamber; the immersion time in the electrolyte sulphate solution as well as its pH and the coating thickness.