Synthesis and non‐isothermal crystallization behavior of poly(ethylene phthalate‐co‐terephthalate)s

A series of poly(ethylene phthalate‐co‐terephthalate)s were synthesized by melt polycondensation of ethylene glycol (EG) with dimethyl phthalate (DMP) and dimethyl terephthalate (DMT) in various proportions. The DMT‐rich polymers were obtained with reasonably high molecular weights, whereas the DMP‐rich polymers were synthesized with relatively low molecular weights due to steric effects associated with the highly kinked DMP monomer. The compositions and thermal properties of the polymers were determined. The copolymers containing DMP in amounts of ≤ 21 mol% were crystallizable, whereas the other polymers were not. All the polymers exhibited a single glass transition temperature. Analysis of the measured glass transition temperatures and crystal melting temperatures confirmed that the DMT‐rich copolymers are random copolymers. The non‐isothermal crystallization behaviors of the DMT‐rich copolymers were investigated by calorimetry and modified Avrami analysis. The Avrami exponents n were found to range from 2.7 to 3.8, suggesting that the copolymers crystallize via a heterogeneous nucleation and spherulitic growth mechanism; that is, the incorporation of DMP units as the minor component does not change the growth mechanism of the copolymers. In addition, the activation energies of the crystallizations of the copolymers were determined; the copolymers were found to have higher activation energies than the PET homopolymer. Polym. Eng. Sci. 44:1682–1691, 2004. © 2004 Society of Plastics Engineers.     

Oxidative coupling of methane over Na+-ZrO2-C1-/Al2O3 catalysts

Oxidative coupling of methane (OCM) was carried out over Na⁺-ZrO₂-Cl /A1[₂O₃ catalysts in a temperature range from 1023 to 1123 K. The catalysts were prepared by impregnating the α- or γ-Al₂O₃ supports with sodium carbonate and/or zirconyl chloride. The OCM activity was examined using the catalysts prepared by three different preparation procedures. The best catalyst was the one prepared by subsequent impregnation of sodium carbonate-preimpregnated γ-Al₂O₃ with a mixed solution of sodium carbonate and zirconyl chloride. It was found that preimpregnated sodium played an important role in reducing the combustion activity of the γ-Al₂O₃. The catalyst with an optimal composition showed the highest C₂ selectivity and yield of 40.8% and 15.1%, respectively. From the X-ray diffraction analysis it was found that tetragonal ZrO₂ was formed and that NaCl existed in the catalysts with relatively high sodium contents.     

Temperature effect on the permeation through poly(2-hydroxyethyl methacrylate) membrane

The temperature dependence of permeability through highly syndiotactic poly(2-hydroxyethyl methacrylate) [P(HEMA)] membrane is reported for highly polar organic solutes such as ureas, methyl substituted ureas and amides, and for NaCl and Na₂SO₄. The membranes used were equilibrated in distilled water at each temperature before measurements. From the linear correlationship between the excess heat capacities, ?C_p^o(excess) in aqueous solution at infinite dilution and the permeability parameter PM^1/3, it is found that the water structure perturbing capability of the polar organic solutes is a controlling factor in the permeation mechanism at relatively low temperature, where P(HEMA) membrane has higher water content and more structured water. In addition, it is found that the poor separation for urea of cellulose acetate membrane in the reverse osmosis practice is due to the higher water structure-breaking capability of urea.     

Electromechanical behavior of hybrid carbon/glass fiber composites with tension and bending

To understand the smart (i.e., good memory) characteristics of hybrid composites of carbon fibers (CFs) and glass fibers (GFs) with epoxy resin as a matrix, the changes in the electrical resistance of composites with tension and on bending were investigated. The electrical resistance behavior of composites under tension changed with the composition of the CF/GF, as well as with the applied strain. The fractional electrical resistance increased slowly with increasing strain within a relatively low strain region. However, with further loading it increased stepwise with the strain according to the fracture of the CF layers. The strain sensitivity of the samples increased with increasing CF weight percentage, and the samples incorporating more than 40 wt % CF showed a strain sensitivity higher than 1.54 for a single CF. The changes in the fractional electrical resistance with bending were not so dominant as those with tension. This difference was attributed to the action of two cancelling effects, which are the increasing and decreasing fractional electrical resistance due to tension and compression with bending, respectively. On recovery from a large applied bending, the fractional electrical resistance decreased slowly with unloading because of the increase of contacts between the fibers that resulted from the reorganization of ruptured CFs during the recovery. Even the composites incorporating a relatively small CF content showed an irreversible electrical resistance with both tension and bending. However, the strain sensitivity being larger with tension than with bending is ascribed to the difference in their mechanical behaviors. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 2447–2453, 2002     

Effect of Additives on the Electromechanical Properties of Pb(Zr,Ti)O3–Pb(Y2/3W1/3)O3 Ceramics

Dielectric and piezoelectric properties of 0.02Pb(Y_2/3W_1/3)O₃ 0.98Pb(Zr0.52Ti0.48)O3 ceramics doped with additives (Nb₂O₅, La₂O₃, MnO₂, and Fe₂O₃) were investigated. The grain sizes of these ceramics decreased with increasing amounts of additives. For additions of MnO₂ and Fe₂O₃, dielectric losses decreased, while for Nb₂O₅ and La₂O₃, these values increased. The maximum values of the mechanical quality factor Q_m were found to be 956 and 975 for additions of 0.9 wt% Fe₂O₃ and 0.7 wt% MnO₂, respectively, but donor dopants (Nb₂O₅ and La₂O₃) did not change the values of Q_m . On the other hand, the piezoelectric constant d₃₃ and the electromechanical coupling factor k_p decreased with additions of MnO₂ and Fe₂O₃, but improved with additions of Nb₂O₅ and La₂O₃.     

Effects of chemical additives on high-field electromechanical properties of PMN–PT–BT ceramics

A chemical additive method using sol–gel reactions was used to modify the composition and resultant properties of a commercially available 0.96(0.91Pb(Mg_1/3Nb_2/3)O₃–0.09PbTiO₃)–0.04 BaTiO₃ (PMN–PT–BT) ceramic. Without an additional ball-mixing process, several combinations of minor additives such as Fe, Ba, Sr, Zn, and Ti were incorporated by the chemical method. Weak- and high-field characteristics including dielectric properties, induced strain and polarization, and associated hystereses were evaluated for the samples sintered at 1200 °C for 4 h. All properties were found to depend on the chemical additives and temperature. Especially, the temperature dependence of high-field characteristics revealed different behavior from that reported for conventionally prepared samples. For example, the samples containing 0.5 wt.% SrO, 0.5 wt.% ZnO, and 0.5 wt.% TiO₂ did not exhibit a transition to piezoelectric behavior at the temperature expected from the dielectric measurements. Overall, the coating process has been successfully used to modify, and in some cases, enhance the high-field characteristics of PMN-based ceramics for electromechanical uses.     

Interfacial adhesion reaction of polyethylene and starch blends using maleated polyethylene reactive compatibilizer

The interfacial reaction of the polyethylene (PE)/starch blend system containing the reactive compatibilizer maleated polyethylene (m‐PE) was directly characterized by Fourier transform infrared (FTIR) spectroscopy. A significant amount of anhydride groups on m‐PE existed as hydrolyzed forms, resulting in a large amount of carboxyl groups. Using a vacuum‐heating‐cell designed in the laboratory, the carboxyl groups were successfully transformed into the dehydrolyzed state (i.e., anhydride group). This result enabled the direct spectroscopic observation of chemical reaction occurring at the interface. For the PE/starch blend system containing m‐PE, the chemical reaction at the interface was verified by the evolution of ester and carboxyl groups in the FTIR spectra. The effect of the reactive compatibilizer on the interfacial morphology was also examined by scanning electron micrography (SEM). Enhanced interfacial adhesion was clearly observed for the blend system containing reactive compatibilizer. Tensile strengths of blend systems containing m‐PE also increased noticeably compared with the corresponding system without compatibilizer. A similar observation was made for the breaking elongation data. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 83: 767–776, 2002     

Boron distribution in a low-alloy steel

Boron distribution in a low-alloy steel (15B26:0.25C-0.29Cr-0.03Ti-0.028Al-0.0016B) has been characterized employing Fission Track Etching (FTE) method. The characteristics of boron distribution with variation of cooling rate after austenitization and through case-hardened depth after carburization were analyzed. Hardenability of 15B26 steel was also evaluated through Jominy-end-quench test and the results are as follows: It was observed that, in austenitized 15B26 steel, boron was distributed uniformly over the whole area of specimen with a little segregation along the austenite grain boundaries at higher cooling rates and boron precipitates were formed in the intergranular as well as transgranular regions at lower cooling rates. Jominy equivalents (HRC 35) of 15B26 steel were fairly increased between the Jominy temperatures of 820°C and 850°C, which might result from the increase of the amount of soluble boron in austenite due to the dissolution of borocarbides between 820°C and 850°C. In carburized 15B26 steel, the different through thickness features of boron distribution from the carburized surface were found; coarse nodular boron precipitates up to the depth of 150 μm; uniform distribution of dissolved boron between 150~650 μm; and segregation of boron atoms along grain boundaries in the regions deeper than 650 μm.     

Corrosion resistance of austenitic stainless steel separator for molten carbonate fuel cell

STS310S and SC-STS310S (simultaneously co-deposited chromium and aluminum onto 310S austenitic stainless steel substrate by pack-cementation process) were used as separator materials on the cathode side of a molten carbonate fuel cell. With the STS310S, corrosion proceeded via three steps; a formation step of unstable corrosion product, a protection step against corrosion until breakaway, and an advance step of corrosion after breakaway. The final corrosion product was LiFeO₂ and the loss of mass was 6.5 mg/cm² after a corrosion test of 480 hr at 650°C. The SC-STS310S showed more effective corrosion resistance, however, than did common STS310S. There was especially no corrosion loss on the SC-STS310S after the 480 hr corrosion test. It is anticipated that it will be very useful as an alternative separator on the cathode side off the MCFC in the future.     

The preparation of tantalum powder using a MR-EMR combination process

In the conventional metallothermic reduction (MR) process used to obtain tantalum powder in batch-type operation, it is difficult to control the morphology and location of the tantalum deposits. In contrast, an electronically mediated reaction (EMR) process is capable of overcoming this difficulty. It has the advantage of being a continuous process, but has the disadvantage of a poor reduction yield. A process known as the MR-EMR combination process is able to overcome the shortcomings of the MR and EMR processes. In this study, an MR-EMR combination process is applied to the production of tantalum powder via sodium reduction of K₂TaF₇. In the MR-EMR combination process, the total charge passed through an external circuit and the average particle size (FSSS) increase as the reduction temperature increases. In addition, the proportion of fine particles (−325 mesh) decreases as the reduction temperature increasess. The tantalum yield improved from 65 to 74% as the reduction temperature increased. Taking into account the charge, impurities, morphology, particle size and yield, a reduction temperature of 1123 K was found to be optimum for the MR-EMR combination process.