Synthesis of uniform microspheres with higher content of 2-hydroxyethyl methacrylate by employing SPG (Shirasu porous glass) emulsification technique followed by swelling process of droplets

Relatively uniform microspheres containing a hydrophilic monomer, 2-hydroxyethyl methacrylate (HEMA), were prepared by employing a swelling method of uniform seed droplets. A uniform seed emulsion composed mainly of styrene (St) was prepared by the Shirasu porous glass (SPG) membrane emulsification technique; this was mixed with a secondary emulsion composed mainly of HEMA/St or HEMA/MMA (methyl methacrylate) prepared by a homogenizer for swelling. The swollen droplets obtained were polymerized at 75°C under a nitrogen atmosphere. The uniform microsphere with a higher content of HEMA was obtained successfully by the swelling method while it failed by a direct emulsification method. The effects of the composition of the oil phase and the inhibitor in the continuous phase on the incorporated fraction of HEMA, the morphology of particles, and monomer conversion were investigated. It was found that the incorporated fraction of HEMA increased with increasing its feed fraction, and more HEMA was incorporated into the microsphere when HEMA/MMA was used as the oil phase of the secondary emulsion rather than HEMA/St. Although the final conversion was very low when the feed fraction of HEMA was higher, it can be increased to more than 80% by using an adequate amount of ethylene glycol dimethacrylate (EGDMA) as a crosslinker and NaNO₂ as an inhibitor in the aqueous phase. Various microspheres with different morphologies such as spherical, snowmanlike, and popcornlike were observed, depending on composition of the oil phase. Furthermore, the porous microsphere with a high content of HEMA was obtained by employing hexanol (HA) as a porogen. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 66: 1325–1341, 1997     

Influence of swelling of noncrystalline regions in silk fibers on modification with methacrylamide

The degrees of swelling of noncrystalline regions of domestic and tussah silk fibers were investigated by measuring the small-angle X-ray scattering intensity of the fibers in wet conditions and analyzing the scattering intensity based on a two-phase model, i.e., crystalline regions and water-swollen noncrystalline regions. The influence of the degree of swelling of noncrystalline regions on the graft treatment of these fibers with methacrylamide was investigated. The changes in the structure caused by the graft treatment were also analyzed using the wide-angle X-ray diffraction measurements. As compared with the tussah silk fibers, the domestic silk fibers showed a larger degree of swelling of the noncrystalline regions, and gained a larger amount of resin by the graft treatment. The crystallites with smaller sizes in the tussah silk fibers were destroyed preferentially by the graft treatment. For the domestic silk fibers, the crystallites were destroyed more seriously and rather homogeneously independent of the crystallite sizes. © 1996 John Wiley & Sons, Inc.     

Fabrication of an atomic resolution low cost STM-SNOM hybrid probe

We derived a simple method to fabricate STM-SNOM hybrid probes obtained from commercial cheap communication optical fibers. The tips are fabricated by a methodology that combines two well-known techniques: the selective attack by a buffered solution and the protected layer chemical etching, in a single new one-step technique. The tailored probes are then sputtered by metal and mounted on a STM setup. The usual difficulties of integrating the optical fiber in the STM head are solved originally with a particular home made mount described in details. We will show that the resulting probes reach atomic resolution on both vertical and horizontal scale, and that the optical imaging is free of artifacts and satisfactory with a lateral resolution in the order of lamda/20, as far as we know the finest resolution obtained with a system based on a hybrid fiber probe. We believe that our methodology is very interesting for its simplicity of realization and for the good resolving power in both SNOM and STM modes.     

Supercritical hydrothermal synthesis and in situ organic modification of indium tin oxide nanoparticles using continuous-flow reaction system

ITO nanoparticles were synthesized hydrothermally and surface modified in supercritical water using a continuous flow reaction system. The organic modification of the nanoparticles converted the surface from hydrophilic to hydrophobic, making the modified nanoparticles easily dispersible in organic solvent. The addition of a surface modifier into the reaction system impacted the crystal growth and particle size as well as dispersion. The particle size was 18 nm. Highly crystalline cubic ITO with a narrow particle size distribution was obtained. The advantages of short reaction time and the use of a continuous reaction system make this method suitable for industrial scale synthesis.     

Influence of asymmetric electrode geometry on an impedance spectrum of a plasma-sprayed thermal barrier coating system

Influence of asymmetric electrode geometry on an impedance spectrum of a plasma-sprayed thermal barrier coating (TBC) system was investigated. The impedance spectrum of the TBC system included impedance of the yttria stabilized zirconia (YSZ) grains, YSZ grain boundaries (negligible), the thermally grown oxide (TGO) and the electrode reaction. In the TBC system with a continuous TGO layer, the impedance of the YSZ grain was measured without influence of asymmetric electrode geometry above 100 kHz. In a frequency range below 100 kHz, asymmetric electrode geometry induced the spread of an electrical conduction region outside an electrode attached on the top coating surface. The impedance of the TGO and the electrode reaction was significantly affected by the asymmetric electrode geometry. The precise interpretation of an impedance spectrum of TBC systems measured under the condition of asymmetric electrode geometry requires further studies on the spread of an electrical conduction region due to decrease in frequency, increase in asymmetry of electrode geometry.     

Effects of cyclic vertical loading on bearing and pullout capacities of piles with continuous helix wing

Laboratory and field tests were conducted to investigate the bearing and pullout capacities of steel piles with a continuous helix wing during cyclic loading. Both continuous helix and straight-sided piles were subjected to monotonic compressive, monotonic tensile, and cyclic reversal loading in the laboratory, while only the continuous helix pile was tested in the field. Both the laboratory and the field tests showed that the bearing and pullout capacities of the continuous helix pile under cyclic reversal loading decreased to approximately 60–80% of those of the pile under monotonic loading, with a larger reduction seen in the laboratory tests. The decrease in resistance was mainly due to the reduction in shaft friction, which was likely to be the result of soil disturbance and loosening around the pile with cyclic loading. The laboratory tests also showed that the tip resistance of the straight-sided pile under cyclic reversal loading was reduced, similarly due to the loosening of the soil, particularly underneath the pile tip. The tip resistance of the continuous helix pile, in contrast, did not degrade with cyclic loading, owing to the presence of the wing immediately above the pile tip that inhibited the loosening of the soil. These findings were supported by similar field test observations.     

Joint strength of Inconel 718 alloy and its improvement by post-weld heat treatment – joint performance and its controlling factors in friction welding of Inconel 718 alloy

The influences of welding parameters on tensile properties of friction-welded joints of Inconel 718 alloy (subjected to a post-weld heat treatment (PWHT) consisting of a solution treatment at 1253 K and double ageing treatments at 993 and 893 K) have been investigated to reveal the controlling factor of the joint performance. All joints obtained were fractured near the bond interface at smaller elongations and area reductions than the base metal on tensile tests, although most of them showed tensile strengths comparable with that of the base metal. The observations of fractured surface and its cross-sectional microstructure suggested that an interfacial fine grain zone including numerous fine Laves phase particles 30–100 nm in size was responsible for a low ductility fracture at shorter friction time and lower friction pressure. As the friction time and pressure were increased, the fine grain zone disappeared, and a reduction in hardness near the bond interface became significant, causing a rather ductile fracture near the bond interface. With an increase in friction time, coarse Laves phase particles, a few micrometres in size remaining near the bond interface increased and they acted as a crack nucleation site of ductile fracture. An increase in the solution treatment temperature during the post-weld heat treatment enhanced the dissolution of the coarse Laves phase in the low-hardness region, and enabled us to obtain joints that were free from unacceptable grain growth and fractured in the base metal at a solution treatment temperature of 1323 K.