Pyrolysis of tertiarybutylphosphine at low pressure

The pyrolysis of tertiarybutylphosphine (TBP) has been studied in the low pressure conditions used for chemical beam epitaxy (CBE). The pyrolysis studies were carried out in low pressure reactors of two different configurations, one of which is a cracker cell designed for use in a CBE system. The reaction products were studied using a quadrupole mass spectrometer. The products observed are accounted for by a reaction mechanism involving homolysis of the parent TBP molecule to produce PH₂ and C₄H₉ radicals. These undergo subsequent reactions to form the stable products C₄H₈, PH₃ and H₂, with smaller amounts of P and P₂ being produced. The production of the sub-hydride PH₂ using this cracker cell design indicates that the use of partially cracked TBP may be a promising technique for reducing the amount of carbon incorporated into the growing epitaxial layer.     

Controlled oxygen incorporation in indium gallium arsenide and indium phosphide grown by metalorganic vapor phase epitaxy

The defect engineering in metalorganic vapor phase epitaxy In_xGa_1-xAs and InP by controlled oxygen doping using diethyl aluminum ethoxide (DEALO) was developed in this study. DEALO doping has led to the incorporation of Al and O, and the compensation of shallow Si donors in In_xGa_1−xAs: Si with 0 ≤ x ≤ 0.25. With the same DEALO mole fraction during growth, the incorporation of Al and O was found to be independent of x, but the compensation of Si donors decreases with increasing In content. Deep level transient spectroscopy analysis on a series of In_xGa_1-xAs: Si. samples with 0 ≤ x ≤ 0.18 revealed that oxygen incorporation led to a set of deep levels, similar to those found in DEALO doped GaAs. As the In composition was increased, one or more of these deep levels became resonant with the conduction band and led to a high electron concentration in oxygen doped In_0.53Ga_0.47As. Low temperature photoluminescence emission measurements at 12K on the same set of samples revealed the quenching of the near-band edge peak, and the appearance of new oxygen-induced emission features. DEALO doping in InP has also led to the incorporation of Al and O, and the compensation of Si donors due to oxygen-induced multiple deep levels.     

Growth of high-quality GaSb by metalorganic vapor phase epitaxy

The growth of nominally undoped GaSb layers by atmospheric pressure metalorganic vapor phase epitaxy on GaSb and GaAs substrates is studied. Trimethylgallium and trimethylantimony are used as precursors for the growth at 600°C in a horizontal reactor. The effect of carrier gas flow, V/III-ratio, and trimethylgallium partial pressure on surface morphology, electrical properties and photoluminescence is investigated. The optimum values for the growth parameters are established. The carrier gas flow is shown to have a significant effect on the surface morphology. The optimum growth rate is found to be 3–8 μm/ h, which is higher than previously reported. The 2.5 μm thick GaSb layers on GaAs are p-type, having at optimized growth conditions room-temperature hole mobility and hole concentration of 800 cm² V⁻¹ s⁻¹ and 3·10¹⁶ cm^-3, respectively. The homoepitaxial GaSb layer grown with the same parameters has mirror-like surface and the photoluminescence spectrum is dominated by strong excitonic lines.     

InSb,GaSb, and GaInSb grown using trisdimethylaminoantimony

GalnSb alloys as well as the constituent binaries InSb and GaSb have been grown by organometallic vapor phase epitaxy using the new antimony precursor trisdimethylaminoantimony (TDMASb) combined with conventional group III precursors trimethylindium (TMIn) and trimethylgallium (TMGa). InSb layers were grown at temperatures between 275 and 425°C. The low values of V/III ratio required to obtain good morphologies at the lowest temperatures indicate that the pyrolysis temperature is low for TDMASb. In fact, at the lowest temperatures, the InSb growth efficiency is higher than for other antimony precursors, indicating the TDMASb pyrolysis products assist with TMIn pyrolysis. A similar, but less pronounced trend is observed for GaSb growth at temperatures of less than 500°C. No excess carbon contamination is observed for either the InSb or GaSb layers. Ga_1-xIn_xSb layers with excellent morphologies with values of x between 0 and 0.5 were grown on GaSb substrates without the use of graded layers. The growth temperature was 525°C and the values of V/III ratio, optimized for each value of x, ranged between 1.25 and 1.38. Strong photoluminescence (PL) was observed for values of x of less than 0.3, with values of halfwidth ranging from 13 to 16 meV, somewhat smaller than previous reports for layers grown using conventional precursors without the use of graded layers at the interface. The PL intensity was observed to decrease significantly for higher values of x. The PL peak energies were found to track the band gap energy; thus, the luminescence is due to band edge processes. The layers were all p-type with carrier concentrations of approximately 10¹⁷ cm³. Transmission electron diffraction studies indicate that the Ga_0.5In_0.5 Sb layers are ordered. Two variants of the Cu-Pt structure are observed with nearly the same diffracted intensities. This is the first report of ordering in GalnSb alloys.     

Selective area epitaxy of CdTe

We have performed selective area epitaxy (SAE) of CdTe layers grown by molecular beam epitaxy using a shadow mask technique. This technique was chosen over other SAE techniques due to its simplicity and its compatibility with multiple SAE patterning steps. Features as small as 50 microns × 50 microns were obtained with sharp, abrupt side walls and flat mesa tops. Separations between mesas as small as 20 microns were also obtained. Shadowing effects due to the finite thickness of the mask were reduced by placing the CdTe source in a near normal incidence position. Intimate contact between the mask and the substrate was essential in order to achieve good pattern definition.     

Gelation of poly(n-butylisocyanate) in benzene

Poly (n-butylisocyanate)-benzene solutions prepared by solubilization at 45°C, followed by aging at room temperature were found to be metastable for months, although, eventually, they separated into a birefringent polymer-rich phase and an isotropic solution. These metastable solutions, as well as isothermally phase-separated biphasic samples, flowed and exhibited dynamic moduli indicative of low polymer connectivity. By contrast samples prepared by a freeze-thaw cycle were uniformly and highly birefringent and showed network (gel) behavior at room temperature. The mechanism of gel formation is most likely the exclusion of the polymer from the benzene crystal during crystallization, forcing the polymer to align and exist at grain boundaries. Films formed from solutions have different moduli than those formed from gels, and are consistent with the proposed mechanism.     

轴端沟槽底部激光强化工艺参数优化研究

分析了选用不同激光能量密度对HT300进行表面强化处理时，材料表面呈现的四种状况；未相变硬化、相变硬化、表面微熔与表面熔凝的金相组织。根据工艺要求，选取相变硬化方法对轴端沟槽底表面进行处理。分析了工件激光处理方法并通过试验研究，寻找轴端沟槽底部激光强化工艺参数；激光功率（P）、光斑直径（D）及扫描速度（V）的优化组合。硬度测试及耐磨性能试验表明：激光相变处理和激光熔凝处理后轴端沟槽底部表面较表面感应淬火硬度分别提高7%和34%，绝对磨损体积分别下降了13%和25%。实践证实，对轴端沟槽底部激光相变硬化处理方法较其他表面处理方法工艺简单，加工工件符合技术要求，试验结果对零件表面处理提供了可靠依据。     

Formation of GaAsP interface layers monitored by reflectance anisotropy spectroscopy

Reflectance anisotropy spectroscopy (RAS) has been used to study As-by-P exchange during metalorganic vapor phase epitaxy. The study focuses on the processes occurring during switching from GaAs to GaInP, especially the effect of purging PH₃ over a GaAs surface. GaAsP/GaAs superlattices of different periodicity were grown and the P-content was determined by high-resolution x-ray diffraction and correlated to the RAS spectra. From the temperature dependence of the P-content, an activation energy of 0.56 eV was estimated for the incorporation mechanism. In addition to the insights into the processes at mixed group-V heterointerfaces, our study demonstrates the reproducibility of RAS transients that thus can be used for process monitoring.     

Determination of the liquidus lines and isotherms of the Hg-Zn-Te system by a modified direct observation method

The modified direct observation method is employed for the determination of the liquidus lines in the (Hg_{1_x}Zn_x)_{1_y}Te_y, ternary system. The liquidus temperatures of the ternary samples of various compositions withx from 0.05 to 0.30 andy from 0.5 to 0.9 are measured. The temperature-composition phase diagrams and some liquidus isotherms are established for this system.     

Two new asterosaponins from the starfish Asterias rubens: application of a cryogenic NMR probe head

We report two new asterosaponins from the Baltic starfish Asterias rubens along with their ¹H and ¹³C NMR data. The compounds were isolated after on‐flow liquid chromatography–NMR–mass spectrometry screening indicated that they had not been identified before. The one‐ and two‐dimensional NMR experiments used to elucidate the structures were recorded using a 5 mm cryogenic probe head. The advantages of cryogenic probes for this kind of examination in comparison with conventional probe heads are discussed. Copyright © 2003 John Wiley & Sons, Ltd.