Anodic chlorination of aniline in N,N-dimethyl-formamide and N,N-dimethylacetamide

A pertinent electrochemical synthesis of 2,4,6-trichloroaniline (TCA) in anhydrous media was studied. The influence of the solvent, the chlorinating reagent, the electricity passed and the nature of the anode material, were investigated. TCA was produced in electrolytic solutions whose solvents were amides with strong nucleophilicity as N,N-dimethylformamide (DMF) and N,N-dimethylacetoamide (DMAc), and was obtained selectively by the controlled potential electrolysis of aniline in the solution containing LiCl. The definition of the experimental conditions corresponding to an optimum and selective electrolysis of TCA was described.     

Liquid film dryout in a boiling channel under flow oscillation conditions

A simple theory was developed to elucidate the influence of sinusoidal oscillation of the inlet flow rate on the occurrence of liquid film dryout in an annular two-phase flow regime in a boiling channel. The theory assumes that the critical heat flux (CHF) under an oscillatory condition can be calculated from values in steady states provided that the effect of axial mixing of the liquid film is appropriately considered. The trends of CHFs calculated using a one-dimensional three-fluid model and those experimentally measured under atmospheric pressure were in reasonable agreement with the proposed theory. However, the CHF values measured under oscillatory conditions were usually higher in the experiment than in the numerical simulation, which indicated that axial liquid transport induced by disturbance waves might enhance axial mixing of the liquid film.     

Liquid film behavior in annular two-phase flow under flow oscillation conditions

Experiments were carried out to investigate the effects of sinusoidal forced oscillation of the inlet flow rate on the time variations of local liquid film thickness and the frequencies of large wave’s passing in steam–water annular two-phase flows. The liquid film thickness oscillated with the same period as the inlet flow rate. The mean film thickness in the thin film regions decreased and approached to an asymptotic value with an increase in the oscillation period of the inlet flow rate. This result was consistent with the experimental results of the occurrence of liquid film dryout under flow oscillation conditions reported in the literature. It was hence considered that the axial liquid transport from the thick to thin film regions mitigates the reduction of the critical heat flux caused by the flow oscillation. It was also found that the wave frequency in the thin film region increased with a decrease in the oscillation period. This observation suggested that the disturbance waves contribute to the enhancements of the liquid transport and consequently the critical heat flux associated with the liquid film dryout under flow oscillation conditions.     

Rate of droplet deposition in steam-water annular flow and effect of a flow obstacle

Deposition rate of droplets in steam-water annular two-phase flow was measured using a 5 mm diameter vertical round tube as a test section. In the experimental conditions tested in this work, the droplet mass transfer coefficient decreased with an increase in the droplet concentration in the gas core flow and with an increase in the length of a deposition section. The dependence on these two parameters agreed fairly well with predictions by available correlations. Placing a small cylindrical tube concentrically in the test section round tube, the effect of a flow obstacle on the deposition rate of droplets was also experimentally investigated. It was found that the obstacle effect was significant and the deposition rate of droplets increased approximately three times in average. The obstacle effect measured in this work was compared with an empirical correlation and a simple mechanistic model that were developed using experimental results of air-water annular flows. Fairly good agreement was achieved in both cases, which would indicate that the mechanism of deposition enhancement induced by the flow obstacle is similar between air-water and steam-water flows.     

Evaluation on plastic deformation property of copper nano-film by nano-scale cantilever specimen

We investigate the elasto-plastic deformation properties of a 20-nm-thick copper (Cu) thin film. A nano-scale cantilever specimen is fabricated from multilayer thin films, where the Cu thin film is sandwiched between a silicon nitride layer and a silicon substrate. During bending, the load, P, and displacement, d, are carefully monitored using an electron microscope, and a distinct non-linearity is observed. The plastic constitutive equation of the Cu thin film, which is assumed to obey a power hardening law (σ = Rεⁿ (σ > σ_y)), is inversely derived by finite element method fitting the experimental results. The residual stress in each layer is experimentally examined, and the effect is included in the inverse analysis. We obtain σ = 3316ε^0.29 [MPa] and a yield stress of 765 MPa for the Cu film. The yield stress is about 10 times higher than that of the bulk, and the exponent is also larger. Moreover, inverse analysis based on the bending experiment data, without considering the residual stress, gives a good approximation of the plastic law. This is because the plastic deformation preferentially takes place at the top and bottom surfaces, where the residual stress is relieved during fabrication of the specimen.     

Voltage-controlled double-resonance quartz oscillator using variable-capacitance diode

In this work, we present a variable-frequency quartz crystal oscillator that is able to oscillate at LC resonance under frequency locking of a quartz crystal resonance, with the frequency tuning realized by variable-capacitance diodes. This circuit shows a steep transition between LC oscillation modes to quartz crystal double-resonance, which shows a characteristic change in the oscillation frequency. Control voltage of this diode is precisely adjusted from the low side to higher values and conversely in the vicinity of the oscillation mode transition. The transition of the oscillation modes is experimentally demonstrated and compared with an algebraic analysis.     

Evaluation of Desulphurization Flux in CaO‐Al2O3‐BaO‐CeO2‐MgO System

The flux of the CaO‐Al₂0₃‐BaO‐CeO₂‐MgO system as a desulphurization flux containing no fluorine for the secondary metallurgy process was evaluated in this study. The flux composition was designed using the eutectic compositions of the binary systems. The melting and desulphurization abilities of the fluxes were evaluated by measuring their liquidus temperatures and the distribution ratios of sulphur between the fluxes and the carbon‐saturated iron or stainless steel. The lowest liquidus temperature of 1325°C was obtained by adding 5.7 mass% MgO to the 80mass%A‐20mass%B flux. (A: 12CaO‐7Al₂O₃, B: BaCeO₃+12mass%Al₂O₃). The distribution ratios of sulphur and sulphide capacities of the fluxes in this study were higher than those of the commercial product of calcium aluminate flux. This means that the CaO‐Al₂O₃‐BaO‐CeO₂‐MgO fluxes developed in this study have higher desulphurization and melting abilities compared with the commercial product of calcium aluminate flux.     

A camera calibration technique using three sets of parallel lines

This paper presents a new method for three-dimensional camera calibration in which the rotation parameters are decoupled from the translation parameters. First, the rotation parameters are obtained by projecting three sets of parallel lines independently of the translation parameters and the imaging distance from the lens to the image plane. The virtual line passing through the image center, which is calculated by perspective projection of a set of parallel lines, depends only on the rotation parameters. Next, the translation parameters and the imaging distance are analytically obtained. Experimental results are used to show how the camera model can be accurately reconstructed in an easily prepared environment.