Fabrication of lead-free piezoelectric (Bi<Subscript>0.5</Subscript>Na<Subscript>0.5</Subscript>)TiO<Subscript>3</Subscript>–BaTiO<Subscript>3</Subscript> ceramics using electrophoretic deposition

Electrophoretic deposition (EPD) process has certain advantages such as it can be applied for a mass production and also can be combined with magnetic crystal alignment technique. In this work, we prepared lead-free 85(Bi_0.5Na_0.5)TiO₃–15BaTiO₃ (85BNT–15BT) piezoelectric ceramics by conventional uniaxial pressing and EPD process. Various conditions were optimized such as suspension media, applied electrical field, and deposition time in order to yield dense green ceramics of 85BNT–15BT composition using EPD process. 85BNT–15BT ceramics prepared using EPD process revealed the Curie temperature of about 250 °C, coercive field of about 30 kV/cm, and piezoelectric constant (d ₃₃) of 75 pC/N. The EPD-processed samples exhibited structural and electrical properties similar to that of the conventionally processed one suggesting the successful fabrication of 85BNT–15BT piezoelectric ceramics by EPD method without composition deviation. This study lays a foundation on the fabrication of Bi-based lead-free piezoelectric ceramics by an alternative route other than the conventionally practiced solid-state reaction method maintaining the similar chemical composition, moreover, leaving a large space to explore more in the future.     

Low-temperature sintering of ZrW2O8–SiO2 by spark plasma sintering

Amorphous ZrW₂O₈ powder and amorphous SiO₂ powder were prepared by a sol–gel process as raw materials, and high-density ZrW₂O₈–SiO₂ were successfully prepared at a much lower temperature of 923 K for a much shorter holding time of 10 min by spark plasma sintering (SPS) method rather than by conventional melt-quenching method. The relative densities of 0.85ZrW₂O₈–0.15SiO₂ and 0.70ZrW₂O₈–0.30SiO₂ were 99.4% and 96.6%, respectively. The combined technique of a sol–gel process and SPS should enable us to prepare the varied types of high-density composites of ZrW₂O₈ without severe thermal cracking caused by melt-quenching. The thermal expansion properties and dielectric properties of ZrW₂O₈–SiO₂ were also investigated.     

Analysis of glycosyl bond cleavage and related isotope effects in collision-induced dissociation quadrupole-time-of-flight mass spectrometry of isomeric trehaloses

The configuration isomers alpha,alpha-, alpha,beta-, and beta,beta-trehalose are distinguishable by a relative ion abundance analysis using collision-induced dissociation MS/MS measurements in electrospray ionization quadrupole-time-of-flight mass spectrometry. The relative abundance of the Y-type fragment ion of alpha,alpha-trehalose is the highest and that of beta,beta-trehalose is the lowest, indicating that alpha-glycosyl bonds cleave more easily than beta-glycosyl bonds. The relative ion abundance depends on both the alpha- and beta-glycosyl linkage type and the number of alpha-glycosyl bonds. The reaction path of glycosyl bond cleavage is calculated computationally using the molecular orbital method in the form of Hartree-Fock theory in conjunction with the 6-31G(d) basis set. The results are consistent with the experimental data. Isotope effects on the fragmentation of the glycosyl bonds are detected in the experiments of the H2O/D2O solvent systems. Furthermore, the isotope effect regarding beta,beta-trehalose is larger than those of alpha,alpha- and alpha,beta-trehalose, indicating that the isotope effect on the beta-glycosyl bond cleavage is larger than that on the alpha-glycosyl bond cleavage. The thermal energy increase in trehalose-d8 molecules over the corresponding trehalose molecules is calculated from the vibrational modes.     

Pressureless sintering and characterization of cordierite/ZrO2 composites

Cordierite/ZrO₂ composites with 5 to 25 wt% ZrO₂ were fabricated by conventional powder mixing and pressureless sintering method. Their densification behavior, microstructure, mechanical and thermal properties were studied. By dispersing 25 wt% (9.57 vol%) ZrO₂, densified cordierite/ZrO₂ composite with a relative density of 98.5% was obtained at an optimum sintering condition of 1440 °C and 2 h. ZrO₂ particles were homogenously dispersed within matrix grains and at the grain boundaries. The intragranular particles were finer than 100 nm and the intergranular particles were coarser. Both fracture strength and toughness could be enhanced more than two times higher, compare to those of monolithic cordierite, by dispersing 25 wt% ZrO₂ into the cordierite matrix. The toughening mechanism in the present composites was mainly attributed to martensitic transformation due to ZrO₂ dispersion. Electronic Publication     

Simple and comprehensive two-dimensional reversed-phase HPLC using monolithic silica columns

Simple and comprehensive two-dimensional (2D)-HPLC was studied in a reversed-phase mode using monolithic silica columns for second-dimension (2nd-D) separation. Every fraction from the first column, 15 cm long (4.6-mm i.d.), packed with fluoroalkylsilyl-bonded (FR) silica particles, was subjected to the separation in the 2nd-D using one or two octadecylsilylated (C(18)) monolithic silica columns (4.6-mm i.d., 3 cm). Monolithic silica columns in the 2nd-D were eluted at a flow rate of up to 10 mL/min with separation time of 30 s that meets the fractionation every 15-30 s at the first dimension (1st-D) operated at a flow rate of 0.4-0.8 mL/min. Three cases were studied. (1) In the simplest scheme of 2D-HPLC, effluent of the 1st-D was directly loaded into an injector loop of 2nd-D HPLC for 28 s, and 2 s was allowed for injection. (2) Two six-port valves each having a sample loop were used to hold the effluent of the 1st-D alternately for 30 s for one 2nd-D column to effect comprehensive 2D-HPLC without the loss of 1st-D effluent. (3) Two monolithic silica columns were used for 2nd-D by using a switching valve and two sets of 2nd-D chromatographs separating each fraction of the 1st-D effluent with the two 2nd-D columns alternately. In this case, two columns of the same stationary phase (C(18)) or different phases, C(18) and (pentabromobenzyloxy)propylsilyl-bonded (PBB), could be employed at the 2nd-D, although the latter needed two complementary runs. The systems produced peak capacity of approximately 1000 in approximately 60 min in cases 1 and 2 and in approximately 30 min in case 3. The three stationary phases, FR, C(18), and PBB, showed widely different selectivity from each other, making 2D separations possible. The simple and comprehensive 2D-HPLC utilizes the stability and high efficiency at high linear velocities of monolithic silica columns.     

Calculating optimal modulation periods to maximize the peak capacity in two-dimensional HPLC

Theoretical calculations are presented to optimize modulation period for maximum total peak capacity in comprehensive two-dimensional HPLC (2D-HPLC) taking into account the effect of modulation on the apparent peak capacity of the first-dimension (1D) separation. Results indicate that modulation periods are most favorable when they are adjusted to approximately 2.2-4 times the standard deviation of a 1D peak in order to avoid excessively short run times at the second dimension (2D). Data are presented that effective peak capacities of several thousand in 60 min can be expected for practical 2D-HPLC conditions, utilizing 1D gradient elution followed by 2D isocratic elution, that remain at approximately 50-70% of the theoretical maximum peak capacity. This work suggests that lower modulation frequencies and longer 2D separation times than previously proposed are favorable under realistic chromatographic conditions, alleviating some practical problems associated with 2D-HPLC.     

Nonlinear effects on spin waves in3He-4He dilute solutions

Spin dynamics of³He-⁴He dilute solution have been studied in the collisionless regime by NMR methods. In cw NMR experiments, we observed spin waves in a magnetic field gradient. The frequency difference between the first mode and the others obeyed a two-thirds power law in the strength of the field gradient. By using a pulsed NMR method, nonlinear spin dynamics were studied. We observed the large amplitude spin waves after an rf pulse. The frequency of each spin-wave mode depended on the tipping angle. By using the parameter determined in the present experiment, the numerical calculated results based on Leggett-Rice theory are in good agreement with the results of the pulsed NMR experiments.     

Grazing exit electron probe microanalysis of submicrometer inclusions in metallic materials

Grazing exit electron probe microanalysis (GE-EPMA) is a new method of EPMA in which characteristic X-rays emitted from only near-surface regions of a specimen are detected at extremely low exit angles near 0 degrees (the grazing exit condition). This technique requires the analytical objects exist on a flat surface. Therefore, the GE-EPMA analysis has been used only for the analysis of particles or a thin film on a flat substrate so that there were only few applications for practical analysis. As a new application, we have carried out GE-EPMA analysis of approximately 0.2-microm inclusions on stainless steel, which appeared to be a projection on the specimen surface with chemical etching. The GE-EPMA quantitative results were in excellent agreement with those of inclusions that were extracted from the stainless steel and analyzed by EPMA with conventional exit condition (30 degrees). This method could be, therefore, applied to the analysis of the submicrometer inclusion in a wide variety of metallic materials if the inclusion appears to be a projection with chemical etching treatment.     

Development of multianode photomultiplier tube

We have developed a multianode photomultiplier tube (MAPMT) which has a sensitive cathode diameter of 36 mm and an anode with 88 segments. The position sensitivity of the tube was studied by using light from a LED and scintillation light from a scintillation-fiber bundle. We observed particle tracks for the first time by using a single photomultiplier tube.