Charge-sensitive deep level transient spectroscopy of helium-ion-irradiated silicon, as-irradiated and after thermal annealing

Electrically active defects in the phosphor-doped single-crystal silicon, induced by helium-ion irradiation under thermal annealing, have been investigated. Isothermal charge-sensitive deep-level transient spectroscopy was employed to study the activation energy and capture cross-section of helium-induced defects in silicon samples. It was shown that the activation energy levels produced by helium-ion irradiation first increased with increasing annealing temperature, with the maximum value of the activation energy occurring at 873K, and reduced with further increase of the annealing temperature. The energy levels of defects in the samples annealed at 873 and 1073K are found to be located near the mid-forbidden energy gap level so that they can act as thermally stable carrier recombination centres.

碳化硅中氦离子高温注入引出的缺陷及其退火行为的光谱研究

6H-SiC single crystal specimens were implanted at 600 K with 100 KeV He ions to three successively increasing fluences and subsequently annealed at different temperatures ranging from 600℃ to 1200℃ in vacuum.After the annealing,the samples were investigated by using Raman scattering spectroscopy and photoluminescence spectrometry,respectively.Both of the two methods showed that the damage induced by helium-ion-implantation in the lattice is closely related to the dose.The thermal annealing brings about reco...中文摘要：对氦(He)离子高温(600K)注入6H-SiC中的辐照缺陷,在阶梯温度退火后演化行为的拉曼光谱和室温光致发光谱的特征进行了分析.这两种方法的实验结果表明,离子注入所产生晶格损伤的程度与注入剂量有关;高温退火导致损伤的恢复,不同注入剂量造成的晶格损伤需要不同的退火温度才可恢复.在阶梯温度退火下呈现出了点缺陷的复合、氦-空位团的产生、氦泡的形核、长大等特性.研究表明:高温(600K)注入在一定剂量范围内是避免注入层非晶化的一个重要方法,为后续利用氦离子注入空腔掩埋层吸杂或者制备低成本、低缺陷密度的绝缘层上碳化硅(SiCOI)材料提供了可能.

碳化硅中氦离子高温注入引入的缺陷及其退火行为的光谱研究

对氦(He)离子高温(600K)注入6H-SiC中的辐照缺陷,在阶梯温度退火后演化行为的拉曼光谱和室温光致发光谱的特征进行了分析.这两种方法的实验结果表明,离子注入所产生晶格损伤的程度与注入剂量有关;高温退火导致损伤的恢复,不同注入剂量造成的晶格损伤需要不同的退火温度才可恢复.在阶梯温度退火下呈现出了点缺陷的复合、氦-空位团的产生、氦泡的形核、长大等特性.研究表明:高温(600K)注入在一定剂量范围内是避免注入层非晶化的一个重要方法,为后续利用氦离子注入空腔掩埋层吸杂或者制备低成本、低缺陷密度的绝缘层上碳化硅(SiCOI)材料提供了可能.

Synthesis and Crystal Structure of a New 3D Copper B-Paradodecatungstate Compound: [Na-2(H2O)(8)][Na-8(H2O)(20)][Cu(en)(2)][W12O42] center dot 3H(2)O

A new polyoxotungstate complex [Na-2(H2O)(8)][Na-8(H2O)(20)][Cu(en)(2)][W12O42] center dot 3 H2O (1) (en = ethylenediamine) has been synthesized in aqueous solution and characterized by elemental analysis, IR spectroscopy and TG analysis, together with a single crystal X-ray diffraction study. In compound 1, the Cu(en)(2)(2+) complex cation links the [W12O42](12-) anions to form a I D chain, and the ID chains are further interconnected with Na-8(H2O)(20)(8+) and Na-2(H2O)(8)(2+) cations to construct a new 3D framework.

Characterization and optimization of AuNPs labeled by Raman reporters on glass based on silver enhancement

In this report, gold nanoparticles (AuNPs) labeled by Raman reporters (AuNPs-R6G) were assembled on glass and used as the seeds to in situ grow silver-coated nanostructures based on silver enhancer solution, forming the nanostructures of AuNPs-R6G@Ag, which were characterized by scanning electron microscopy (SEM) and UV-visible spectroscopy. More importantly, the obtained silver-coated nanostructures can be used as a surface enhancement Raman scattering (SERS) substrate. The different SERS activities can be controlled by the silver deposition time and assembly time of AuNPs-R6G on glass. The results indicate that the maximum SERS activity could be obtained on AuNPs-R6G when these nanostructures were assembled on glass for 2 h with silver deposition for 2 min.

Carbon Nanotube/Silica Coaxial Nanocable as a Three-Dimensional Support for Loading Diverse Ultra-High-Density Metal Nanostructures: Facile Preparation and Use as Enhanced Materials for Electrochemical Devices and SERS

In this paper, we have reported a very simple strategy (combined sonication with sol-gel techniques) for synthesizing well-defined silica-coated carbon nanotube (CNT) coaxial nanocable without prior CNT functionalization. After functionalization with NH2 group, the CNT/silica coaxial nanocable has been employed as a three-dimensional support for loading ultra-high-density metal or hybrid nanoparticles (NPs) such as gold NPs, Au/Pt hybrid NPs, Pt hollow NPs, and Au/Ag core/shell NPs. Most importantly, it is found that the ultra-high-density Au/Pt NPs supported on coaxial nanocables (UASCN) could be used as enhanced materials for constructing electrochemical devices with high performance. Four model probe molecules (O-2, CH3OH, H2O2, and NH2NH2) have been investigated on UASCN-modified glassy carbon electrode (GCE). It was observed that the present UASCN exhibited high electrocatalytic activity toward diverse molecules and was a promising electrocatalyst for constructing electrochemical devices with high performance. For instance, the detection limit for H2O2 with a signal-to-noise ratio of 3 was found to be 0.3 mu M, which was lower than certain enzyme-based biosensors.

Synthesis and characterization of polyethylene chains grafted onto the sidewalls of single-walled carbon nanotubes via copolymerization

Polyethylene (PE) chains grafted onto the sidewalls of SWCNTs (SWCNT-g-PE) were successfully synthesized via ethylene copolymerization with functionalized single-walled carbon nanotubes (f-SWCNTs) catalyzed by rac-(en)(THInd)(2)ZrCl2/ MAO. Here f-SWCNTs, in which alpha-alkene groups were chemically linked on the sidewalls of SWCNTs, were synthesized by Prato reaction. The composition and microstructure of SWCNT-g-PE were characterized by means of H-1 NMR, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analyses (TGA), field-emission scanning electron microscope (FESEM), and transmission electron microscope (TEM). Nanosized cable-like structure was formed in the SWCNT-g-PE, in which the PE formed a tubular shell and several SWCNTs bundles existed as core. The formation of the above morphology in the SWCNT-g-PE resulted from successfully grafting of PE chains onto the surface of SWCNTs via copolymerization. The grown PE chains grafted onto the sidewall of the f-SWCNTs promoted the exfoliation of the mass nanotubes. Comparing with pure PE, the physical mixture of PE/f-SWCNTs and in situ PE/SWCNTs mixture, thermal stability, and mechanical properties of SWCNT-g-PE were higher because of the chemical bonding between the f-SWCNTs and PE chains.

Syntheses, crystal structures and magnetic properties of two heterometallic coordination polymers

Two heterometallic chain coordination polymers with the chemical formula {[Cu2Mn2L2(CH3OH)(H2O)] center dot 0.5CH(3)OH center dot 0.5CH(3)CH(2)OH}(n) (1) and {[Cu2Co2L2(H2O)(2)] center dot H2O}(n) (2) have been synthesized and characterized by IR, UV spectroscopy and single-crystal X-ray structural analysis, where H4L = 2-hydroxy-3-[(E)-({2-[(2-hydroxybetizoyl)amino]ethyl}imino)methyl] benzoic acid. Magnetic measurements showed that the two compounds exhibit antiferromagnetic coupling exchange interactions, and satisfactory fittings to the observed magnetic susceptibility data were obtained by assuming a linear four-spin arrangement with two isotropic magnetic exchange interactions.

Optical spectroscopy properties of KMgF3 : Eu2+ nanocrystals and powder synthesized by microemulsion and solvothermal process

Nanocrystals and powders of KMgF3 doped with Eu2+ were synthesized by the microemulsion method and the solvothermal process, respectively. The emission and excitation spectra of KMgF3:Eu2+ phosphors were measured and compared with those of the samples synthesized through a solid. state reaction, Bridgman-Stockbarger method, and mild hydrothermal technique. The KMgF3: Eu2+ samples synthesized by means of the microemulsion method and the solvothermal process show only a sharp emission peak located at 360 nm, in the emission spectra, which arises from the f -> f(P-6(1/2)-> S-8(1/2)) transition of Eu2+. The broad emission bands appear at 420 nm,,which arises from Eu2+ <- O2- cannot be observed(in the mild hydrothermal and single crystal samples, the emission peak at 420 nm besides the emission of Eu2+ at 360 nm is observed). In the excitation spectrum of the KMgF3: Eu2+ samples synthesized by the microemulsion method and the solvothermal process, the excitation peaks show an intensive blue shift. The blue shift can he attributed to the lower oxygenic content in the KMgF3: Eu2+ samples synthesized by the microemulsion method and the solvothermal process.

Synthesis, electrocatalytic properties and crystal structure of a new organic-inorganic hybrid constructed from dodecamolybdophosphoric acid and benzotriazole

A new compound, (C6H6N3)(7)((PMo12O40)-O-m)(PMo(v)Mo(11)(m)O40) (.) 2CH(3)CH(2)OH (.) 5H(2)O, was synthesized and characterized by means of elemental analyses, IR spectroscopy, H-1 NMR spectroscopy and single crystal X-ray diffraction. This is the first example of benzotriazole-polyoxometalates species. The compound crystallized in a triclinic space group P (1) over bar with a = 1. 8378 (4) nm. b = 1. 9078 (4) nm. c = 2.1037 (4) nm. alpha = 63.41 (3)degrees. beta = 64.31 (3)degrees. gamma = 68.38 (3)degrees. V = 5.803 (2) nm(3). Z = 2. R-1 = 0.0486, wR(2) = 0.1357. The X-ray crystallographic study showed that the crystal structure was constructed by electrostatic interactions and hydrogen bonds between dodecamolybdophosphorate anions and protonated benzotriazole cations. The electrochemical behavior and the reduction of nitrite and hydrogen peroxide clectrocatalyzed by the title compound were studied.

Self-assembled monolayer of polyoxometalate on gold surfaces: Quartz crystal microbalance, electrochemistry, and in-situ scanning tunneling microscopy study

A new kind of inorganic self-assembled monolayer (SAM) was prepared by spontaneous adsorption of polyoxometalate anion, AsMo11VO404-, onto a gold surface from acidic aqueous solution. The adsorption process, structure, and electrochemical properties of the AsMo11VO404- SAM were investigated by quartz crystal microbalance (QCM), electrochemistry, and scanning tunneling microscopy (STM). The QCM data suggested that the self-assembling process could be described in terms of the Langmuir adsorption model, providing the value of the free energy of adsorption at -20 KJ mol(-1). The maximum surface coverage of the AsMo11VO404- SAM on gold surface was determined from the QCM data to be 1.7 x 10(-10) mol cm(-2), corresponding to a close-packed monolayer of AsMo11VO404- anion. The analysis of the voltammograms of the AsMo11VO404- SAM on gold electrode showed three pairs of reversible peaks with an equal surface coverage of 1.78 x 10(-10) mol cm(-2) for each of the peaks, and the value was agreed well with the QCM data. In-situ STM image demonstrated that the AsMo11VO404- SAM was very uniform and no aggregates or multilayer could be observed. Furthermore, the high-resolution STM images revealed that the AsMo11VO404- SAM on Au(lll) surface was composed of square unit cells with a lattice space of 10-11 Angstrom at +0.7 V (vs Ag\AgCl). The value was quite close to the diameter of AsMo11VO404- anion obtained from X-ray crystallographic study. The surface coverage of the AsMo11VO404- SAM on gold electrode estimated from the STM image was around 1.8 x 10(-10) mol cm(-2), which was consistent with the QCM and electrochemical results.

NORMAL COORDINATE TREATMENT OF LEU(5)-ENKEPHALIN IN THE CRYSTAL-STATE

Vibrational studies on the neuropentapeptide Leu5-enkephalin were performed for the crystal state where different specific conformations can arise. In the present case, the peptide adopts a double fused folded conformation (beta-turn), the presence of which in the crystal state is directly related to the nature of the solvent used for its crystallization. This study completes other work relating to similar conformations of isolated molecules. It can be seen that specific interactions in the crystal state perturb to a large extent the vibrational relationships between the amide frequencies and the specific sets of dihedral angles characteristic of the particular type of turn. The tyrosyl moiety and its frequency dependence on its hydrogen bond state was especially investigated both for the Fermi resonance and the hydroxyl bending modes.

A fully integrated multi-channel detector for electron spectroscopy

Langstaff, David; Bushell, A.; Chase, T.; Evans, D.A., (2005) 'A fully integrated multi-channel detector for electron spectroscopy', Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 238 pp.219-223 RAE2008 Synchrotron Radiation in Materials Science ? Proceedings of the 4th Conference on Synchrotron Radiation in Materials Science 4th Conference on Synchrotron Radiation in Materials Science

Vibrational spectra and crystal structure of the di-amino acid peptide cyclo(L-Met-L-Met): Comparison of experimental data and DFT calculations

Experimental Raman and FT-IR spectra of solid-state non-deuterated and N-deuterated samples of cyclo(L-Met-L-Met) are reported and discussed. The Raman and FT-IR results show characteristic amide I vibrations (Raman: 1649 cm-1, infrared: 1675 cm-1) for molecules exhibiting a cis amide conformation. A Raman band, assigned to the cis amide II vibrational mode, is observed at sim1493 cm-1 but no IR band is observed in this region. Cyclo(L-Met-L-Met) crystallises in the triclinic space group P1 with one molecule per unit cell. The overall shape of the diketopiperazine (DKP) ring displays a (slightly distorted) boat conformation. The crystal packing employs two strong hydrogen bonds, which traverse the entire crystal via translational repeats. B3-LYP/cc-pVDZ calculations of the structure of the molecule predict a boat conformation for the DKP ring, in agreement with the experimentally determined X-ray structure. Copyright © 2009 John Wiley & Sons, Ltd.

Development of sampling methods for Raman analysis of solid dosage forms of therapeutic and illicit drugs

The results of a study aimed at determining the most important experimental parameters for automated, quantitative analysis of solid dosage form pharmaceuticals (seized and model 'ecstasy' tablets) are reported. Data obtained with a macro-Raman spectrometer were complemented by micro-Raman measurements, which gave information on particle size and provided excellent data for developing statistical models of the sampling errors associated with collecting data as a series of grid points on the tablets' surface. Spectra recorded at single points on the surface of seized MDMA-caffeine-lactose tablets with a Raman microscope (lambda(ex) = 785 nm, 3 mum diameter spot) were typically dominated by one or other of the three components, consistent with Raman mapping data which showed the drug and caffeine microcrystals were ca 40 mum in diameter. Spectra collected with a microscope from eight points on a 200 mum grid were combined and in the resultant spectra the average value of the Raman band intensity ratio used to quantify the MDMA: caffeine ratio, mu(r), was 1.19 with an unacceptably high standard deviation, sigma(r), of 1.20. In contrast, with a conventional macro-Raman system (150 mum spot diameter), combined eight grid point data gave mu(r) = 1.47 with sigma(r) = 0.16. A simple statistical model which could be used to predict sigma(r) under the various conditions used was developed. The model showed that the decrease in sigma(r) on moving to a 150 mum spot was too large to be due entirely to the increased spot diameter but was consistent with the increased sampling volume that arose from a combination of the larger spot size and depth of focus in the macroscopic system. With the macro-Raman system, combining 64 grid points (0.5 mm spacing and 1-2 s accumulation per point) to give a single averaged spectrum for a tablet was found to be a practical balance between minimizing sampling errors and keeping overhead times at an acceptable level. The effectiveness of this sampling strategy was also tested by quantitative analysis of a set of model ecstasy tablets prepared from MDEA-sorbitol (0-30% by mass MDEA). A simple univariate calibration model of averaged 64 point data had R-2 = 0.998 and an r.m.s. standard error of prediction of 1.1% whereas data obtained by sampling just four points on the same tablet showed deviations from the calibration of up to 5%.