Assignment of chemical shifts in benzohydroxamic acid and structure of its silylated derivatives by 15N enrichment

¹⁵N isotopic enrichment was necessary for the unequivocal assignment of the ¹H NMR lines to the protons in the NH–OH fragment of benzohydroxamic acid, BHXA, C₆H₅CONHOH, in dry dimethyl sulfoxide solutions. The assignment [δ(NH) = 11.21, δ(OH) = 9.01, ¹J(¹⁵N,¹H) = 102.2 Hz, ²J(¹⁵N,¹H) <1.5 Hz], which is opposite to that used by other authors, confirms the assignment extended to BHXA by Brown and co‐workers from the spectra of acetohydroxamic acid. The enrichment allowed also assignment of the ²⁹Si lines in the spectra of disilylated benzohydroxamic acid, (Z)‐tert‐butyldimethylsilyl N‐tert‐butyldimethylsilyloxybenzoimidate (2) and (Z)‐tert‐butyldiphenylsilyl N‐tert‐butyldiphenylsilyloxybenzoimidate (3), and confirmed structure of the monosilylated products, N‐tert‐butyldiphenylsilyloxybenzamide (4) and N‐tert‐butyldiphenylsilyloxy benzoimidic acid (5). Copyright © 2003 John Wiley & Sons, Ltd.     

SiGe (Ge-dot) heterojunction phototransistors for efficient light detection at 1.3–1.55 μm

The aim of this work is to develop a Si/SiGe HBT-type phototransistor with several Ge dot layers incorporated in the collector, in order to obtain improved light detectivity at 1.3–1.55 μm. The MBE grown HBT detectors are of n–p–n type and based on a multilayer structure containing 10 Ge-dot layers (8 ML in each layer, separated by 60 nm Si spacer) in the base-collector junction. The transistors were processed for normal incidence or with waveguide geometry where the light is coupled through the edge of the sample. The measured breakdown voltage, BV_ceo, was about 6 V. Compared to a p–i–n reference photodiode with the same dot layer structure, photoconductivity measurements show that the responsivity is improved by a factor of 60 for normal incidence at 1.3 μm. When the light is coupled through the edge of the device, the detectivity is even further enhanced. The measured photo-responsivity is more than 100 and 5 mA/W at 1.3 and 1.55 μm, respectively.     

超短脉冲激光微束对细胞作用的研究

本文详细地介绍了我们自己设计和安装的一个Nd:YAG超短脉冲激光微束系统,该系统分成二个部分:激光源和显微镜。由电光调Q非稳腔Nd:YAG激光倍频后得到355nm紫外光进入显微镜并由物镜聚焦。同时,这超短脉冲激光微束照射在细胞上并且在细胞上产生一个可以自恢复的小孔。在文中我们还讨论了超短脉冲激光微束与细胞之间作用效应及机理。     

Flicker noise in degenerately doped Si single crystals near the metal-insulator transition

In this paper we report some of the important results of experimental investigations of the flicker noise near the metal-insulator (MI) transition in doped silicon single crystals. This is the first comprehensive work to study low-frequency noise in heavily doped Si over an extensive temperature range (2 K<T<500 K). The measurements of conductance fluctuations (flicker noise) were carried out in the frequency range 10⁻²<f<4 × 10¹ Hz in single crystalline Si across the MI transition by doping with phosphorous and boron. The magnitude of noise in heavily doped Si is much larger than that seen in lightly doped Si over the whole temperature range. The extensive temperature range covered allowed us to detect two distinct noise mechanisms. At low temperatures (T<100 K) universal conductance fluctuations (UCF) dominate and the spectral dependence of the noise is determined by dephasing the electron from defects with two-levels (TLS). At higher temperatures (T>200 K) the noise arises from activated defect dynamics. As the MI transition is approached, the 1/f spectral power, typical of the metallic regime, gets modified by the presence of discrete Lorentzians which arise from generation-recombination process which is the characteristic of a semiconductor.     

Chemical synthesis of p-type nanocrystalline copper selenide thin films for heterojunction solar cells

Nanocrystalline thin films of copper selenide have been grown on glass and tin doped-indium oxide substrates using chemical method. At ambient temperature, golden films have been synthesized and annealed at 200 °C for 1 h and were examined for their structural, surface morphological and optical properties by means of X-ray diffraction (XRD), scanning electron microscopy and UV-vis spectrophotometry techniques, respectively. Cu_2−xSe phase was confirmed by XRD pattern and spherical grains of 30 ± 4 - 40 ± 4 nm in size aggregated over about 130 ± 10 nm islands were seen by SEM images. Effect of annealing on crystallinity improvement, band edge shift and photoelectrochemical performance (under 80 mW/cm² light intensity and in lithium iodide electrolyte) has been studied and reported. Observed p-type electrical conductivity in copper selenide thin films make it a suitable candidate for heterojunction solar cells.     

Investigation of sulfonated poly(ether ether ketone sulfone)/heteropolyacid composite membranes for high temperature fuel cell applications

The sulfonated poly(ether ether ketone sulfone) (SPEEKS)/heteropolyacid (HPA) composite membranes with different HPA content in SPEEKS copolymers matrix with different degree of sulfonation (DS) were investigated for high temperature proton exchange membrane fuel cells. Composite membranes were characterized by Fourier transfer infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). FTIR band shifts suggested that the sulfonic acid groups on the copolymer backbone strongly interact with HPA particles. SEM pictures showed that the HPA particles were uniformly distributed throughout the SPEEKS membranes matrix and particle sizes decreased with the increment of copolymers' DS. The holes were not found in SPEEKS‐4/HPA30 (consisting of 70% SPEEKS copolymers with DS = 0.8 and 30% HPA) composite membrane after composite membranes were treated with boiling water for 24 h. Thermal stabilities of the composite membranes were better than those of pure sulfonated copolymers membranes. Although the composite membranes possessed lower water uptake, it exhibited higher proton conductivity for SPEEKS‐4/HPA30 especially at high temperature (above 100 °C). Its proton conductivity linearly increased from 0.068 S/cm at 25 °C to 0.095 S/cm at 120 °C, which was higher than 0.06 S/cm of Nafion 117. In contrast, proton conductivity of pure SPEEKS‐4 membrane only increased from 0.062 S/cm at 25 °C to 0.078 S/cm at 80 °C. At 120 °C, proton conductivity decreased to poor 0.073 S/cm. The result indicated that composite membranes exhibited high proton conductivity at high temperature. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 44: 1967–1978, 2006     

Electrocatalytic activity of ordered intermetallic PtSb for methanol electro-oxidation

Ordered intermetallic PtSb had been synthesized by arc-melted and then sintering treatment. The electro-oxidation of liquid methanol on PtSb was investigated at room temperature by cyclic voltammetry and chronoamperometry. The results are compared to those at a polycrystalline platinum electrode surface. It was found that PtSb intermetallic was catalytically more active than pure platinum according to the onset potential and current density. X-ray diffraction (XRD) and XPS technologies had been used to investigate the crystal structure and electron effect.     

Nuclear spin-lattice relaxation mechanisms in kaolinite confirmed by magic-angle spinning

Spin-lattice relaxation mechanisms in kaolinite have been reinvestigated by magic-angle spinning (MAS) of the sample. MAS is useful to distinguish between relaxation mechanisms: the direct relaxation rate caused by the dipole-dipole interaction with electron spins is not affected by spinning while the spin diffusion-assisted relaxation rate is. Spin diffusion plays a dominant role in ¹H relaxation. MAS causes only a slight change in the relaxation behavior, because the dipolar coupling between ¹H spins is strong. ²⁹Si relaxes directly through the dipole-dipole interaction with electron spins under spinning conditions higher than 2 kHz. A spin diffusion effect has been clearly observed in the ²⁹Si relaxation of relatively pure samples under static and slow-spinning conditions. ²⁷Al relaxes through three mechanisms: phonon-coupled quadrupole interaction, spin diffusion and dipole-dipole interaction with electron spins. The first mechanism is dominant, while the last is negligibly small. Spin diffusion between ²⁷Al spins is suppressed completely at a spinning rate of 2.5 kHz. We have analyzed the relaxation behavior theoretically and discussed quantitatively. Concentrations of paramagnetic impurities, electron spin-lattice relaxation times and spin diffusion rates have been estimated.     

A Novel Method to Synthesize Polyorganozircosilazane

A new kind of polyorganozircosilazane as Si/Zr/C/N-based ceramic precursor was synthesized from the condensation reaction of hexamethyleyclotrisilazane lithium salts(D3^NLi）and zirconium tetrachloride(ZrCl4).In the presence of N,N,N’,N’-tetramethyl ethylene diamine(TMEDA),polyorganozircosilazane was obtained in high yield.