Surface morphology of He-implanted single-crystalline silicon

Single-crystalline Si (100) samples were implanted with 30 keV He2+ ions to doses ranging from 2.0x10(16) to 2.0x10(17) ions/cm(2) and subsequently thermally annealed at 800 degrees C for 30min. The morphological change of the samples with the increase of implantation dose was investigated using atomic force microscopy (AFM). It was found that oblate-shaped blisters with an average height around 4.0nm were found on the 2.0 x 10(16) ions /cm(2) implanted sample surface; spherical-shaped blisters with an average height wound 10.0nm were found on the 5.0 x 10(16) ions/cm(2) implanted sample surface; strip-shaped and conical cracks were observed on the sample He-implanted to a dose of 1.0 X 10(17) ions /cm(2). Exfoliations occurred on the sample surface to a dose of 2.0 x10(17) ions /cm(2). Mechanisms underlying the surface change were discussed.

Electrochemical fabrication of single-crystalline and polycrystalline Au nanowires: the influence of deposition parameters

We report the electrochemical growth of gold nanowires with controlled dimensions and crystallinity. By systematically varying the deposition conditions, both polycrystalline and single-crystalline wires with diameters between 20 and 100 nm are successfully synthesized in etched ion-track membranes. The nanowires are characterized using scanning electron microscopy, high resolution transmission electron microscopy, scanning tunnelling microscopy and x-ray diffraction. The influence of the deposition parameters, especially those of the electrolyte, on the nanowire structure is investigated. Gold sulfite electrolytes lead to polycrystalline structure at the temperatures and voltages employed. In contrast, gold cyanide solution favours the growth of single crystals at temperatures between 50 and 65 degrees C under both direct current and reverse pulse current deposition conditions. The single-crystalline wires possess a [110] preferred orientation.

Color center formation in silica glass induced by high energy Fe and Xe ions

Silica glass samples were implanted with 1.157 GeV Fe-56 and 1.755 GeV Xe-136 ions to fluences range from 1 x 10(11) to 3.8 x 10(12) ions/cm(2). Virgin and irradiated samples were investigated by ultraviolet (UV) absorption from 3 to 6.4 eV and photoluminescence (PL) spectroscopy. The UV absorption investigation reveals the presence of various color centers (E' center, non-bridging oxygen hole center (NBOHC) and ODC(II)) appearing in the irradiated samples. It is found that the concentration of all color centers increase with the increase of fluence and tend to saturation at high fluence. Furthermore the concentration of E' center and that of NBOHC is approximately equal and both scale better with the energy deposition through processes of electronic stopping, indicating that E' center and NBOHC are mainly produced simultaneously from the scission of strained Si-O-Si bond by electronic excitation effects in heavy ion irradiated silica glass. The PL measurement shows three emissions peaked at about 4.28 eV (alpha band), 3.2 eV (beta band) and 2.67 eV (gamma band) when excited at 5 eV. The intensities of alpha and gamma bands increase with the increase of fluence and tend to saturation at high fluence. The intensity of beta band is at its maximum in virgin silica glass and it is reduced on increasing the ions fluence. It is further confirmed that nuclear energy loss processes determine the production of alpha and gamma bands and electronic energy loss processes determine the bleaching of beta band in heavy ion irradiated silica glass. (c) 2009 Elsevier B.V. All rights reserved.

An etched porous interface for on-line capillary electrophoresis-based two-dimensional separation system

The construction and evaluation of an on-column etched fused-silica porous junction for on-line coupling of capillary isoelectric focusing (CIEF) with capillary zone electrophoresis (CZE) are described. Where two separation columns were integrated on a single piece of fused-silica capillary through the etched similar to4 to 5-mm length porous junction along the capillary. The junction is easily prepared by etching a short section of the capillary wall with HF after removing the polyimide coating. The etched section becomes a porous glass membrane that allows only small ions related to the background electrolyte to pass through when high voltage is applied across the separation capillary. The primary advantages of this novel porous junction interface over previous designs (in which the interface is usually formed by fracturing the capillary followed by connecting the two capillaries with a section of microdialysis hollow fiber membrane) are no dead volume, simplicity, and ruggedness, which is particularly well suited for an on-line coupling capillary electrophoresis-based multiple dimensional separation system. The performance of the 2D CIEF-CZE system constructed by such an etched porous junction was evaluated by the analyses of protein mixtures.

Heat capacity and thermodynamic properties of crystalline ornidazole (C7H10ClN3O3)

The molar heat capacities of 1-(2-hydroxy-3-chloropropyl)-2-methyl-5-nitroimidazole (Ornidazole) (C7H10CIN3O3) with purity of 99.72mol% were measured with an adiabatic calorimeter in the temperature range between 79 and 380K. The melting-point temperature, molar enthalpy Delta(fus)H(m), and entropy, Delta(fus)S(m), of fusion of this compound were determined to be 358.59 +/- 0.04K, 21.38 +/- 0.02 kJ mol(-1) and 59.61 +/- 0.05 J K-1 mol(-1), respectively, from fractional melting experiments. The thermodynamic function data relative to the reference temperature (298.15 K) were calculated based on the heat capacities measurements in the temperature range from 80 to 380 K. The thermal stability of the compound was further investigated by DSC and TG. From the DSC curve an intensive exothermic peak assigned to the thermal decomposition of the compound was observed in the range of 445-590 K with the peak temperature of 505 K. Subsequently, a slow exothermic effect appears when the temperature is higher than 590 K, which is probably due to the further decomposition of the compound. The TG curve indicates the mass loss of the sample starts at about 440K, which corresponds to the decomposition of the sample. (C) 2003 Elsevier B.V. All rights reserved.

Calorimetric study and thermal analysis of crystalline nicotinic acid

As one primary component of Vitamin B-3, nicotinic acid [pyridine 3-carboxylic acid] was synthesized, and calorimetric study and thermal analysis for this compound were performed. The low-temperature heat capacity of nicotinic acid was measured with a precise automated adiabatic calorimeter over the temperature rang from 79 to 368 K. No thermal anomaly or phase transition was observed in this temperature range. A solid-to-solid transition at T-trs = 451.4 K, a solid-to-liquid transition at T-fus = 509.1 K and a thermal decomposition at T-d = 538.8 K were found through the DSC and TG-DTG techniques. The molar enthalpies of these transitions were determined to be Delta(trs)H(m =) 0.81 kJ mol(-1), Delta(fus)H(m) 27.57 kJ mol(-1) and Delta(d)H(m) = 62.38 kJ mol(-1), respectively, by the integrals of the peak areas of the DSC curves.

Low-temperature heat capacity and thermodynamic properties of crystalline carboxin (C12H13NO2S)

Carboxin was synthesized and its heat capacities were measured with an automated adiabatic calorimeter over the temperature range from 79 to 380K. The melting point, molar enthalpy (Delta(fus)H(m)) and entropy (Delta(fus)S(m)) of fusion of this compound were determined to be 365.29 +/- 0.06K, 28.193 +/- 0.09 kJ mol(-1) and 77.180 +/- 0.02 J mol(-1) K-1, respectively. The purity of the compound was determined to be 99.55 mol% by using the fractional melting technique. The thermodynamic functions relative to the reference temperature (298.15 K) were calculated based on the heat capacity measurements in the temperature range between 80 and 360 K. The thermal stability of the compound was further investigated by differential scanning calorimetry (DSC) and thermogravimetric (TG) analysis. The DSC curve indicates that the sample starts to decompose at ca. 290degreesC with the peak temperature at 292.7degreesC. The TG-DTG results demonstrate the maximum mass loss rate occurs at 293degreesC corresponding to the maximum decomposition rate. (C) 2003 Elsevier B.V All rights reserved.

Low-temperature heat capacity and thermodynamic properties of crystalline 2-chloro-5-trichloromethylpyridine

The low-temperature heat capacities of 2-chloro-5-trichloromethylpyridine were measured with a high-precision automated adiabatic calorimeter in the temperature range from 80 K to 345 K. A solid-liquid phase transition was observed from 318.57 K to 327.44 K with peak temperature 324.67 K; the molar enthalpy and entropy of phase transition, DeltaH(m) and DeltaS(m), were determined to be 14.50 +/-0.02 kJ mol(-1) and 44.66 +/- 0.07 kJ K-1 mol(-1), respectively. The thermal stability was investigated through thermogravimetric analysis (TG). The TG and DTG results reveal that 2-chloro-5-trichloromethylpyridine starts to lose mass at 332 K due to evaporation and completely changes into vapour at 483 K under the present experimental conditions.

Synthesis of chiral stationary phases with radical polymerization reaction of cellulose phenylcarbamate derivatives and vinylized silica gel

Cellulose phenylcarbamate derivatives having methacrylate groups were synthesized with regioselective and non-regioselective procedures. These derivatives were chemically immobilized onto a vinylized silica gel, respectively, via a radical co-polymerization reaction. The immobilization was efficiently attained using a small amount of AIBN. The chiral recognition abilities of the prepared chiral stationary phases (CSPs) were evaluated by HPLC resolution of test enantiomers. It was observed that most of the enantiomers were completely resolved with markedly high column efficiency of 30,000-40,000 plates per metre for the eluted peaks. The effect of the amount of methacrylolyl chloride used for preparation on resolution was investigated. A direct comparison of the chiral recognition ability was made on the regioselectively and non-regioselectively prepared CSPs. In addition, the chemically bonded-type of CSPs were found to be relatively stable with addition of solvents such as tetrahydrofuran (THF) and chloroform into the mobile phase, which can lead to the dissolution of cellulose derivatives on the coated CSPs. Thus the choice of solvents used as the mobile phase is greatly extended and better resolution of several test enantiomers was observed on the prepared CSPs with THF and chloroform as a composition in the mobile phase. The batch-to-batch and run-to-run reproducibility was also discussed on the newly prepared CSPs. (C) 2004 Elsevier B.V. All rights reserved.

Unilamellar liposomes covalently coupled on silica gel for liquid chromatography

Silica gel was used as a support for the covalent coupling of liposomes, which could overcome drawbacks of soft gel beads in column efficiency and separation speed. The influences of the concentration of added dimethylaminopyridine and reaction time on the chloroformate activation reaction of silica gel were investigated. Temperature and pH for covalent coupling of liposomes on the activated silica gel were also optimized. Experimental results indicated that the stability of the covalently coupled liposome columns was obviously superior to that of the noncovalently coated liposome columns but the selectivity of both columns was basically identical. Separation and analysis of a crude extract of a traditional Chinese medicine Ligusticum Wallichii and a mixture of small peptides on both columns further support this conclusion.