Distribution of carbon contamination in MgAl2O4 spinel occurring during spark-plasma-sintering (SPS) processing: I – Effect of heating rate and post-annealing

Carbon contamination from the carbon paper/dies during spark-plasma-sintering (SPS) processing was examined in the MgAl₂O₄ spinel. The carbon contamination sensitively changes with the heating rate during the SPS processing. At the high heating rate of 100 °C/min, the carbon contamination having organized structures occurred over almost the entire area from the surface to deep inside the SPSed spinel disk. In contrast, at the slow heating rate of 10 °C/min, the carbon contamination having disordered structures occurred only around the surface area. The carbon phases transform into high pressure CO/CO₂ gases by post-annealing in air and lead to pore formation along the grain junctions. The pore formation significantly occurs at the high heating rate due to the large amount of the contaminant carbon phases. This suggests that if once the carbon contamination was formed in the materials, it is very difficult to remove the carbon phases from the materials.     

Crosslinked acrylic pressure‐sensitive adhesives. II. Effect of humidity on the crosslinking reaction

The effect of humidity during storage on the crosslinking reactions of isocyanate groups was investigated with attenuated total reflectance Fourier transform infrared spectroscopy with pressure‐sensitive adhesives composed of poly[ethyl acrylate‐co‐(2‐ethylhexyl acrylate)‐co‐(2‐hydroxyethyl methacrylate)] as a base resin and polyisocyanate as a crosslinker. A peak‐resolving analysis of the amide II region revealed four bands. According to an analysis of the Fourier transform infrared spectra of the model compounds, these four bands were assigned to free urethane linkages, hydrogen‐bonded urethane linkages, free urea linkages, and hydrogen‐bonded urea linkages. As expected, storage under humid conditions led to the formation of free and hydrogen‐bonded urea linkages corresponding to the promotion of isocyanate consumption. Peak resolution of the amide II region was found to be a reasonable way of monitoring urethane and urea linkages during crosslinking reactions. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 3039–3045, 2003     

High performance liquid chromatographic separation of diacylglycerol acetates to quantitate disaturated species of lung phosphatidylcholine

A high-performance liquid chromatographic (HPLC) separation of diacylglycerol acetates to quantitatite disaturated species of lung phosphatidylcholine (PC) was studied. The diacylglycerol acetates were applied on a reversed phase column, eluted by an isocratic solvent, acetonitrile/isopropanol/water (35:15:1, v/v/v) at a flow rate of 1 ml/min, and detected by differential refractometry (RI). This isocratic HPLC method was useful to separate disaturated species from the others of lung PC. The quantitative analysis of the molecular species separated by HPLC was studied by RI detection. Chroamtograms obtained by RI detection and radioactivity determination of diacylglycerol [³H]acetates prepared by [³H]acetic anhydride were almost identical. The RI detector responsed in the same degree for different, authentic standards of diacylglycerol acetates. The detection limit with RI detection was about 30 nmoles. Molecular species of PCs from human lung and carcinoma tissues were analyzed by this HPLC method. The contents of disaturated species were very similar to those reported previously. These results indicate that RI detection is very useful in the nmole range for the quantitative analysis among the molecular species containing disaturated species.     

Comparison of activities in selective catalytic reduction of NOx by C3H8 over Co/MFI, Fe/MFI, and H/MFI zeolite catalysts

The Co/MFI(SiO₂/Al₂O₃ = 30) were prepared by a precipitation method with NaOCl in alkali solutions exhibited high activities to N₂ at 250 °C for the selective catalytic reduction (SCR) of NO_x. These catalysts showed two UV–vis bands at 700 and 400 nm, indicating the presence of octahedral Co(III) as well as tetrahedral Co(II). The high SCR activity over such Co(III, II)/MFI(30) seems to come from Co(III)---O moieties. The Co(II)MFI(30) catalysts prepared from Co(II)Cl₂ exhibited low SCR activities due to the presence of tetrahedral Co(II) ions in MFI. Less CO formation occurred over Co/MFI catalysts. The Fe/MFI(30) catalyst exhibited high activity due to the presence of some Fe---O species in MFI but more amount of CO were produced during SCR. H/MFI(30) catalyst exhibited a good SCR activity. However, more amount of carbonaceous deposits were produced on it. The correlation between acid concentration and SCR activity was discussed over H/MFIs.     

Fabrication of a poly-Si thin-film transistor with storage capacitor

The fabrication process of a low-temperature poly-Si thin-film transistor (TFT) with a storage capacitor was studied. The atmospheric-pressure chemical-vapour deposited SiO₂ protected the buried indium tin oxide (ITO) from reduction by a pure H₂ plasma treatment that was essential for the effective improvement of the poly-Si TFT characteristics. Thus, a storage capacitor with an ITO (picture electrode)-SiO₂-ITO (buried common electrode) structure was successfully fabricated. The poly-Si TFT with a channel width/length W/L ratio of 5 drove a 3 pF storage capacitor in 2 μs, and it showed superior driverability for LCD use. The TFT also had good hold characteristics under illumination for the realization of grey-scale representation.     

InxGa1−xAs ohmic contacts to n-type GaAs with a tungsten nitride barrier

Significant reduction of the contact resistance of In_0.7Ga_0.3As/Ni/W contacts (which were previously developed by sputtering in our laboratory) was achieved by depositing a W₂N barrier layer between the Ni layer and W layer. The In_0.7Ga_0.3 As/Ni/W₂N/W contact prepared by the radio-frequency sputtering technique showed the lowest contact resistance of 0.2 Ωmm after annealing at 550°C for 10 s. This contact also provided a smooth surface, good reproducibility, and excellent thermal stability at 400°C. The polycrystalline W₂N layer was found to suppress the In diffusion to the contact surface, leading to improvement of the surface morphology and an increase in the total area of the In_xGa−As between metal and the GaAs substrate. These improvements are believed to reduce the contact resistance.     

Superconductivity in the tetragonal phase of La1.9Bi0.1CuO4+δ annealed under high oxygen pressure

We have investigated the relation between the crystal structure and superconductivity in La_1.9Bi_0.1CuO_4+δ , in which the phase separation observed in La₂CuO_4+δ is suppressed. A phase diagram in theT?δ plane is given for La_1.9Bi_0.1CuO_4+δ with excess oxygen. For very smallδ values, the crystal structure is orthorhombic, and an orthorhombic-tetragonal phase transition occurs markedly atδ ～ 0.03 in the measured temperature range between 13 and 293 K. Superconductivity is observed in the range of 0.04<δ<0.11. This is clear evidence thathigh-T _c superconductivity also appears in the tetragonal phase.     

Preparation of polyimide-epoxy composites

The formation of a three dimensional network of crosslinked epoxy leads all unmodified epoxies to have inherent brittleness and relatively low degradation temperatures. Polyimides, on the other hand, are widely used for applications that require high degrees of flexibility and thermal resistance. Here, we have focused on the preparation of epoxy systems cured with polyamic acids instead of traditional amino-group-containing hardening agents. The cure behavior and potential reaction mechanisms of EPON 828 resin and polyamic acid mixtures were evaluated by DSC and TGA. Thermal analysis showed a complex reaction sequence taking place in the mixture and also determined the extent of reaction of the polyamic acid with itself and the competitive reaction of the polyamic acid with the epoxy. The compositions of the mixtures were varied to see the dependence of the cure behavior on component concentrations. Solutions of the two components did not phase separate and also phase separation was not apparent either optically or microscopically in the cured samples. This phase behavior was attributed to a unique in situ reaction. A novel solvent system for the polyamic acid precursor was also used.