Ultrasound‐activated Knoevenagel condensation of malononitrile with carbonylic compounds catalysed by alkaline‐doped saponites

α,β‐Unsaturated nitriles have been synthesized by Knoevenagel condensation of a carbonylic compound with malononitrile, assisted by sonochemical irradiation. Two alkaline‐promoted clays (Li⁺‐ and Cs⁺‐exchanged saponites) have been employed as catalysts. The influence of the carbonylic compound (benzaldehyde or cyclohexanone) and the use of a solvent on the catalytic activity have been studied. Remarkable increase in the conversion values has been found when the reaction is activated by ultrasound, as compared with the thermal activation. In this green, solvent‐free procedure, α,β‐unsaturated nitriles have been produced in very high yields (97%) when the Cs⁺‐saponite is used as catalyst. Copyright © 2004 Society of Chemical Industry     

Investigation of texture effect on visual colour difference evaluation

The texture effect on visual colour difference evaluation was investigated in this study. Five colour centers were selected and textured colour pairs were generated using scanned textile woven fabrics and colour‐mapping technique. The textured and solid colour pairs were then displayed on a characterized cathode ray tube (CRT) monitor for colour difference evaluation. The colour difference values for the pairs with texture patterns are equal to 5.0 CIELAB units in lightness direction. The texture level was represented by the half‐width of histogram, which is called texture strength in this study. High correlation was found between texture strength and visual colour difference for textured colour pairs, which indicates that an increasing of 10 units of texture strength in luminance would cause a decreasing of 0.25 units visual difference for the five colour centers. The ratio of visual difference between textured and solid colour pairs also indicates a high parametric effect of texture. © 2005 Wiley Periodicals, Inc. Col Res Appl, 30, 341–347, 2005; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/col.     

Nutrient removal performance of an anaerobic–anoxic–aerobic process as a function of influent C/P ratio

The laboratory scale anaerobic–anoxic–aerobic (A²O) process fed with synthetic brewage wastewater was designed to investigate the effects of changing feed C/P ratio on the performance of biological nutrient removal (BNR) processes. In the experiment, the influent chemical oxygen demand (COD) concentration was kept at approximately 300 mg L^?1 while the total phosphorus concentration was varied to obtain the desired C/P ratio. Results showed that when the C/P ratio was lower than 32, phosphorus removal efficiency increased as C/P ratio increased linearly, while when the C/P ratio was higher than 32, the P removal efficiency was maintained at 90–98%, and effluent P concentration was lower than 0.5 mg L^?1. However, regardless of the C/P ratio, excellent COD removal (90% or higher) and good total nitrogen removal (75–84%) were maintained throughout the experiments. It was also found that very good linear correlation was obtained between COD uptake per unit P released in the anaerobic zone and C/P ratio. In addition, the P content in the wasted activated sludge increased with the decrease in the C/P ratio. Based on the results, it was recommended that the wastewater C/P ratio and its effects be incorporated into BNR design and operational procedures, appropriate C/P ratios were used to achieve the effluent treatment goals. Copyright © 2005 Society of Chemical Industry     

Colloidal silica removal in coagulation processes for wastewater reuse in a high-tech industrial park.

Four experiments of coagulation and flocculation were conducted to investigate the characteristics of colloidal silica removal in a high-tech industrial wastewater treatment plant for reclamation and reuse of the effluent. Experimental results illustrated that poly-aluminium chloride (PACl) showed higher performances on colloidal silica removal than alum. Interestingly, the two coagulants demonstrated the same capacity on silica removal. The specific silica removal capacity was approximately 0.135 mg SiO2/mg Al2O3 when the dosage of coagulants was in the range 30-150 mg/L Al2O3. In addition, the silica was reduced significantly at the condition of pH above 8. Experimental data implied that precipitation of aluminium flocs was the major mechanism for colloid silica removal in PACl and alum coagulation, besides, charge adsorption was also important for improving removal efficiency. Moreover, the addition of polyacrylic acid (PAA) as a flocculant could slightly advance silica removal in the PACl coagulation. The combined PACl/PAA/flocs coagulation was effective for the removal of colloidal silica, soluble COD, and turbidity and also suitable as a pretreatment unit in wastewater reclamation and reuse processes.     

Effect of specimen size and loading conditions on spalling of concrete

Different qualities of concrete have been fire tested using different geometries of the specimens as well as different load levels and load configurations. The main objective with the study was to examine a test methodology consisting of a full‐scale test and different small scale‐tests for determining the probability of spalling and the amount of spalling of fire exposed concrete structures. A reference specimen was defined as a one‐sided fire exposed slab with the dimensions 1800 × 1200 mm² giving an exposed area of 1500 × 1200 mm². A number of concrete qualities with different probabilities for spalling, were tested using the reference specimen. These tests showed that the reference specimens worked well giving the expected test results. Small specimens were manufactured in different shapes with the same concrete as the one used in the reference tests. These small specimens were tested either at the same time as the reference specimens in the large furnace or afterwards on a small‐scale furnace where the fire exposed surface was 450 × 360 mm². The test results clearly show the increased probability and the increased amount of spalling by using external compressive loading. The results also show that by using pre‐stress through bars or wires the load can be lost due to heating of the bars/wires which results in a decreased amount of spalling. The boundary of the specimen also affects the amount of spalling. The spalling around the edges was in all tests less than the spalling on the central parts of the exposed area. It could also be noted that the spalling did not pass completely through any of the specimens. The reason for this is probably that the water/vapour could migrate out from the unexposed surface of the specimen. Copyright © 2006 John Wiley & Sons, Ltd.     

Detection of failure sites by focused ion beam and nano-probing in the interconnect of three-dimensional stacked circuit structures

Focused ion beam (FIB) and nano-probing were applied for failure analysis of three-dimensional stacked circuits with copper through-silicon-vias between the stacked chips. The failure analysis was done after high temperature storage and thermal cycling tests. Passive voltage contrast in FIB allowed to pinpoint the open sites. FIB cross-sections showed the presence of opens at the bottom of the copper vias. The failure cause was suspected to be an interlayer particle, which was confirmed by optical profilometry. Nano-probing was used on another sample to pinpoint the failure location through the measurement of the local resistance within the daisy chains. The failure was traced out to be related with surface contamination.     

Biaxiale Ermüdung reibrührgeschweißter Strukturelemente

Biaxial fatigue of friction stir welded stiffened panels Within the framework of the European WelAir project, cruciform specimens made from stiffening FSW overlap joints were fatigued in the DLR biaxial test rig. To resemble the loading situation of pressurized fuselage structures, proportional loading without any phase shift, but with different load ratios λ between the loading components in both directions was applied.Natural crack initiation and subsequent crack growth were governed by the stiffness gradient caused by introducing the stringer. Cracks initiated and propagated at run‐in and run‐out locations in a direction perpendicular to the weld seam. The shortest fatigue life was observed for uniaxial loading in welding direction (λ = 0). An additional stress component perpendicular to the joint line (λ > 0) resulted in a higher number of cycles to failure. Similar to single stringer panels, increasing the load ratio also increased the number of cycles to failure for FSW clip‐stringer structural members, but additionally gives a different location of the fatal crack.     

N-Type Field-Effect Transistors Using Multiple Mg-Doped ZnO Nanorods

Nanorod field-effect transistors (FETs) that use multiple Mg-doped ZnO nanorods and a SiO₂ gate insulator were fabricated and characterized. The use of multiple nanorods provides higher on-currents without significant degradation in threshold voltage shift and subthreshold slopes. It has been observed that the on-currents of the multiple ZnO nanorod FETs increase approximately linearly with the number of nanorods, with on-currents of ~1 muA per nanorod and little change in off-current (~4times10^-12). The subthreshold slopes and on-off ratios typically improve as the number of nanorods within the device channel is increased, reflecting good uniformity of properties from nanorod to nanorod. It is expected that Mg dopants contribute to high n-type semiconductor characteristics during ZnO nanorod growth. For comparison, nonintentionally doped ZnO nanorod FETs are fabricated, and show low conductivity to compare with Mg-doped ZnO nanorods. In addition, temperature-dependent current-voltage characteristics of single ZnO nanorod FETs indicate that the activation energy of the drain current is very low (0.05-0.16 eV) at gate voltages both above and below threshold     

The flame retardant mechanism of polyolefins modified with chalk and silicone elastomer

This paper presents the current understanding of the flame retardant mechanism of Casico?. The study includes the flame retardant effect of each individual component: ethylene–acrylate copolymer, chalk and silicone elastomer, as well as the formation of an intumescent structure during heating. The flame retardant properties were investigated by cone calorimetry and oxygen index tests. To obtain insight into the flame retardant mechanism, heat treatment under different conditions has also been performed. The results indicate that the flame retardant mechanism of Casico is complex and is related to a number of reactions, e.g. ester pyrolysis of acrylate groups, formation of carbon dioxide by reaction between carboxylic acid and chalk, ionomer formation and formation of an intumescent structure stabilized by a protecting char. Special emphasis is given to the formation of the intumescent structure and its molecular structure as evaluated from ¹³C MAS‐NMR and ²⁹Si MAS‐NMR, ESCA and XRD analysis. After treatment at 500°C the intumescent structure consists mainly of silicon oxides and calcium carbonate and after treatment at 1000°C the intumescent structure consists of calcium silicate, calcium oxide and calcium hydroxide. Copyright © 2003 John Wiley & Sons, Ltd.