Synthesis of nano-polycrystalline diamond from glassy carbon at pressures up to 25 GPa

ABSTRACT

Nano-polycrystalline diamond (NPD) with various grain sizes has been synthesized from glassy carbon at pressures 15–25?GPa and temperatures 1700–2300°C using multianvil apparatus. The minimum temperature for the synthesis of pure NPD, below which a small amount of compressed graphite was formed, significantly increased with pressure from ～1700°C at 15?GPa to ～1900°C at 25?GPa. The NPD having grain sizes less than ～50?nm was synthesized at temperatures below ～2000°C at 15?GPa and ～2300°C at 25?GPa, above which significant grain growth was observed. The grain size of NPD decreases with increasing pressure and decreasing temperature, and the pure NPD with grain sizes less than 10?nm is obtained in a limited temperature range around 1800–2000°C, depending on pressure. The pure NPD from glassy carbon is highly transparent and exhibits a granular nano-texture, whose grain size is tunable by selecting adequate pressure and temperature conditions.     

Estimation of growth rate in unidirectionally solidified multicrystalline silicon by the growth-induced striation method

Multicrystalline silicon was grown by unidirectional solidification method using the accelerated crucible rotation technique. The application of the accelerated crucible rotation technique in unidirectional solidification method induced growth striations across the axial direction of the grown crystal. This striation pattern was observed from carbon concentration distribution, obtained by using Fourier transform infrared spectroscopy. The generated striation pattern was found to be weak and discontinuous. Some striations were absent, probably due to back melting, caused during each crucible rotation. From the growth striations and applied time period in crucible rotation, the growth rate was estimated by using Fourier transformation analysis.     

Base-free oxidative homocoupling of arylboronic esters

Base-free oxidative homocoupling reaction of arylboronic esters has been found to proceed using a catalytic amount of a palladium-1,3-bis(diphenylphosphino)propane (DPPP) complex under an oxygen atmosphere, affording a variety of biaryls in modest to excellent yields. Even arylboronic esters bearing a base-sensitive functional group are applicable to the reaction.     

Spectroscopic study on the crystal growth in gas evaporation: emission and absorption spectra from Cu smoke

Optical emission and absorption spectra from a growth zone in Cu smoke were measured by using a quartz prism spectrograph and a single-grating spectrophotometer. Atomic lines of Cu, band systems of Cu₂ were observed. Two new band systems with 0–0 band heads at 252.88 and 238.79 nm were found. The continuous spectra due to Rayleigh scattering by fine particles were also observed. Variations of density of various species as a function of vertical position were revealed.     

Palladium-catalyzed synthesis of poly(bromoalkoxy- and bromoalkanoyloxymethylsiloxane)s from poly(hydromethylsiloxane)s

Palladium-catalyzed synthesis of poly(bromoalkoxymethyl- and bromoalkanoyloxymethylsiloxane)s from poly(hydromethylsiloxane)s was studied. Treatment of poly(hydromethylsiloxane)s with mixtures of allyl bromide and cyclic ethers in the presence of a catalytic amount of PdCl₂ gave the corresponding poly[(bromoalkoxy)methylsiloxane]s in good yield. A similar reaction with γ-butyrolactone produced poly[(bromobutanoyloxy)methylsiloxane], although the polymer was highly moisture-sensitive and could not be separated from the reaction mixture. Transformation of the bromoalkoxy unit in the resulting siloxane polymer into an aminoalkoxy group was also examined.     

Influence of extended π-conjugation units on carrier mobilities in conducting polymers

Carrier mobilities in thin films of copolymers with repeat units consisting of oligothiophenes bridged by Si atoms are measured over a range of doping levels, where the numbers of thienylenes in the repeat unit are 7, 8, 10, 12, and 14. The mobilities for these polymer films increased with the increase in doping level and the mobility enhancement followed an increasing order of the π-conjugation length. The magnitude of the mobility increase for the Si polymer comprising 14 thiophene units reached ca. 10⁴, implying that this π-conjugation length is almost sufficient to reproduce transport properties of polythiophenes.     

Chemo-enzymatic Synthesis of Novel Oligo-N-acetyllactosamine Derivatives having a β(1-4)–β(1-6) Repeating Unit by Using Transition State Analogue Substrate

Chitinase-catalyzed hydrolytic and transglycosylating behavior of 1,2-oxazoline derivative of N-acetyllactosamine (LacNAc-oxa) 1 has been investigated. An extremely rapid hydrolysis (ring-opening of the oxazoline moiety) could be observed, suggesting that 1 behaves as a transition state analogue substrate for chitinase A1 (Bacillus circulans WL-12). This disaccharide monomer 1 was found to polymerize under basic conditions, giving rise to novel oligosaccharides having a β(1-4)–β(1-6) repeating unit in the main chain. The degree of polymerization of the resulting oligosaccharides was up to 5. This is the first example of enzymatic glycosylation reaction forming a β(1-6) bond catalyzed by chitinase.     

Conductive characteristics of radical‐bearing polythiophenes using a microcomb‐shaped electrode

The electric conductivity of π‐conjugated and radical‐bearing polymers, i.e., polythiophenes bearing pendant galvinoxyl and phenoxyl radical groups, was measured using a microcomb‐shaped electrode. The electric conductivity was found to be enhanced by the radical content in the polymer. The infrared (IR) and Raman spectroscopies suggested a structural change from an aromatic form to a quinoid one in the polythiophene backbone by the phenoxyl radical generation. The effect of the pendant galvinoxyl radical's unpaired electron on the electric conductivity of the polythiophene was discussed by comparing the conductivity of a radical‐bearing polystyrene and a polythiophene mixed with low‐molecular radical molecules. Copyright © 2007 John Wiley & Sons, Ltd.     

Direct Visualization of Electromagnetic Microfields by Superposition of Two Kinds of Electron Holograms

A new electron holographic method is presented to directly visualize pure phase objects such as electromagnetic microfields, which is achieved by superposition of two kinds of electron holograms. The method is very simple and is twice as sensitive as the conventional double-exposure electron holography and the four-electron-wave interference. Using this technique, an electric field around a charged latex sphere and a magnetic field around a barium ferrite particle have been directly observed.     

Polymeric organosilicon systems. XVII. Synthesis and photochemical and conducting properties of poly[o-and m-(disilanylene)phenylene]s

Poly[o-(tetramethyldisilanylene)phenylene] ( 2a ), poly[o-(1,2-dimethyldiphenyldisilanylene)-phenylene] ( 2b ), poly[m-(tetramethyldisilanylene)phenylene] ( 2c ), and poly[m-(1,2-dimethyldiphenyldisilanylene)phenylene] ( 2d ) were prepared by the sodium condensation reaction of the corresponding 1,2-and 1,3-bis (chlorosilyl)benzenes in toluene. Irradiation of thin films of 2a-2d in air resulted in a rapid decrease of absorption maxima in the ultraviolet region. The photolysis of 2b and 2d in benzene afforded photodegradation products with low molecular weights. When thin films of 2b and 2d were doped with antimony pentafluoride vapor, films which have conductivities of semi-conductor level were obtained. © 1993 John Wiley & Sons, Inc.