Synthesis and structural characterization of novel,fluorinated poly(phthalazinone ether)s containing perfluorophenylene moieties

The synthesis and structural characterization of a series of novel, fluorinated poly(phthalazinone ether)s containing perfluorophenylene moieties are described. The monomers, 4‐(4′‐hydroxyaryl)phthalazin‐1(2H)‐ones ( 2a – 2d ), were conveniently and efficiently synthesized from phenols and phthalic anhydride in two steps via 2‐(4′‐hydroxybenzoyl)benzoic acids, which were first obtained by the Friedel–Crafts reaction in good yields and with high stereoselectivity and were then converted into 2a – 2d by fusion with hydrazine. All the polymers were prepared by nucleophilic aromatic substitution (S_NAr) polycondensation between the compounds perfluorobiphenyl and 4‐(4′‐hydroxyaryl)phthalazin‐1(2H)‐ones ( 2a ‐ 2d ). The resulting fluorinated polymers were readily soluble in common organic solvents (e.g., CHCl₃, tetrahydrofuran, dimethylformamide, dimethyl sulfoxide, N‐methylpyrrolidone, etc.) at room temperature. Their weight‐average molecular weights and the polydispersities ranged from (7.96–18.25) × 10³ to 1.31–2.71, respectively. Their glass‐transition temperatures varied from 213 to 263 °C. They were all stable up to 390 °C both in air and in argon. The 5% weight‐loss temperatures of these polymers in air and argon ranged from 393–487 to 437–509 °C, respectively. Wide‐angle X‐ray diffraction studies indicated they were all amorphous and could be attributed to the presence of kink nonplanar moiety, phenyl phthalazinone along the polymer backbone. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 42: 925–932, 2004     

<Emphasis Type="Italic">Comment on</Emphasis>¶Low temperature specific heat of blue bronze K <Emphasis Type="Bold">0.30</Emphasis>MoO <Emphasis Type="Bold">3</Emphasis>, by J. Odin,J.C. Lasjaunias,K. Biljaković, K. Hasselbach,and P. Monceau

Eur. Phys. J. B 24, 315 (2001) Here we comment on a recently published paper on the presence of a phason contribution in the low temperature heat capacity data of the charge-density-wave compounds K_0.3MoO₃ and (TaSe₄)₂I. We have shown that the anomaly in the C _P / T ³ data reported by Odin et al. is straightforwardly interpreted in terms of low energy phonon modes resulting from the peculiar topology of these compounds. Received 21 February 2002 Published online 19 July 2002     

Amorphous Fe–Mg alloy thin films: magnetic properties and atomic vibrational dynamics

Amorphous (a-) Fe _x Mg_1?x alloys are interesting materials for the investigation of non-Debye-like low-energy vibrational excitations. We have prepared a-Fe _x Mg_1?x alloy thin films (0.3 ≤ × ≤0.7) by vapour quenching. The amorphous state was confirmed by conversion electron Mössbauer spectroscopy between 4.2–300 K, and the x- and temperature-dependence of the isomer shift and hyperfine magnetic field was measured. For x= 0.6 and 0.7, magnetic ordering occurs below ~150 K. The atomic vibrational density of states, g(E), was determined by nuclear resonant inelastic scattering, providing clear evidence for the non-Debye-like low-energy vibrational excitations.     

Sulfur Concentration in Nanoporous Alumina Membrane

Nanoporous alumina membrane prepared by anodic oxidation using sulfuric acid electrolyte was subjected to TG-DTA and X-ray Photoelectron Spectroscopy (XPS or ESCA) to further study the distribution of sulfur. In XPS study, Ar⁺ ion bombardment was performed on the sample to etch the surface at a rate of 3 nm min^-1. As a result, sulfur was found to be concentrated within a depth of 3nm from the surface. The S content of the surface was found to be 2.7±0.5 wt%, and that at a depth of ca. 3 nm and ca. 10 nm was found to be as low as about 0.6±0.11 wt% (5.37±1.0 wt%→ 1.26±0.2wt% SO₂). In TG-DTA, the mass loss of 7.3% was in fair agreement with that calculated on XPS results (7.1±1.2%). This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal coefficient of linear expansion of non-crystalline chalcogenides in the As-S-Se-Te-I system

The object of the paper is an investigation of the glasses of the (As₂S₃)_x(AsSe_0.5Te_0.5I)_100-x. type for 65≤;x≤;95, using methods of thermomechanical analysis. Values of the thermal coefficients of linear expansion in solid and visco-plastic phase were determined. it was shown that introducing arsenic-sulfide in glass-matrix AsChI, i.e. (AsSe_0.5Te_0.5I), leads to an increasing stability of these glasses. The characteristic temperatures of softening Tg and the temperature of the beginning of deformation t_w increase by increasing content of As₂S₃. The analytical forms of dependence of four significant physical values α_g, α_l, Tg, Tw, as a function of As₂S₃ content in the structure of glasses were fitted. This revised version was published online in July 2006 with corrections to the Cover Date.     

非晶态合金催化剂用于二甲基紫脲酸加氢反应

二甲基紫脲酸加氢反应;nicob/白炭黑催化剂;非晶态合金催化剂     

聚苯乙烯非晶区结构的RDF研究

本文介绍了以X-射线衍射法测定非品区结构的径向分市函数RDF方法，并将其应用于聚苯乙烯（PS）非晶区的结构研究．     

代铬刷镀层的耐腐蚀机理的考察

对新型的代铬刷镀层Ni-Fe-W-P-S进行了耐腐蚀性能机理的分析研究。用扫描电镜(SEM)、透射电镜(TEM)、扫描隧道显微镜(STM)、X射线衍射及电子能谱(XPS)等的分析表明，基体组织为非品结构是代铬刷镀层优异耐腐蚀性的主要原因.     

Study of the Crystallization of an Aromatic Poly-ether-ketone (PK99) by Calorimetric and X-ray Analysis

An analysis of the crystallization behaviour of a new poly(aryl-ether-ether-ketone-ketone), PK99, by differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) is presented. Isothermal crystallization TG were obtained in the whole range between the glass transition temperature (T _g) and the melting temperature (T _m) as a consequence of the slow crystallization kinetics stemming from the closeness of these transitions. The calorimetric results, compared with WAXD data, were applied to determine the theoretical melting temperature and crystallization enthalpy. The DSC and WAXD data were combined in order to calculate the total amount of the crystallizable fraction of the polymer, and a model was proposed to explain the difference between the fractions of crystallinity observed with these techniques. The thermal and X-ray data were also correlated with different lamellar morphologies arising from the crystallization conditions. Finally, DSC experiments on the crystallized sample were used to detect the presence of a rigid amorphous phase which does not relax at T _g. This revised version was published online in July 2006 with corrections to the Cover Date.     

Performance of SuSi: a method for generating atomistic models of amorphous polymers based on a random search of energy minima

The performance of a recently developed method to generate representative atomistic models of amorphous polymers has been investigated. This method, which is denoted SuSi, can be defined as a random generator of energy minima. The effects produced by different parameters used to define the size of the system and the characteristics of the generation algorithm have been examined. Calculations have been performed on poly(L,D-lactic) acid (rho = 1.25 g/cm3) and nylon 6 (rho = 1.084 g/cm(3)), which are important commercial polymers.