~(29)S双质子的同时发射

<正>近年来,双质子发射的现象被广泛研究。~(29)S核最外层两个质子处于2s1/2轨道,可能存在这种奇特的行为。先前的实验表明,~(29)S+~(28)Si的总反应截面有着异常大的值。这意味着~(29)S中最后2

Search for signature inversion in the pi i(13/2) circle times upsilon i1(3/2) bands in Au-182,Au-184,Au-186

Search for low-spin signature inversion in the pi i(13/2) circle times nu i(13/2) bands in odd-odd Au-182,Au-184,Au-186 has been conducted through the standard in-beam gamma-spectroscopy techniques. The experiments for Au-182 and 186Au have been performed in the Japan Atomic Energy Agency (JAEA) via the Sm-152(Cl-35,5n)Au-182 and Yb-172(F-19,5n)Au-186 reactions, respectively. A study of Au-184 has been made using a multi-detector array GASP in LNL, Italy, via the Tb-159(Si-29,4n)Au-184 reaction. The pi i(13/2) circle times nu i(13/2) bands in these three nuclei have been identified and extended up to high-spin states. In particular, the inter-band connection between the pi i(13/2) nu i(13/2) band and the ground-state band in 184 Au has been established, leading to a firm spin-and-parity assignment for the pi i(13/2) circle times nu i(13/2) band. The low-spin signature inversion is found in the pi i(13/2) circle times nu i(13/2) bands in Au-182,Au-184,Au-186 according to our spin-assignment and the signature crossing observed at high-spin states.

Search for signature inversion in the pi i(13/2)circle times nu i(13/2) bands in Au-182,Au-184,Au-186

Search for low-spin signature inversion in the pi i(13/2) circle times nu i(13/2) bands in odd-odd Au-182,Au-184,Au-186 has been conducted through the standard in-beam gamma-spectroscopy techniques via the Sm-152(Cl-35,5n) Au-182, Yb-172(F-19,5n) (186)An, and Tb-159(Si-29,4n) (184)An reactions, respectively. The pi i(13/2) circle times nu i(13/2) bands in these three nuclei have been identified and extended up to high-spin states. In particular, the inter-band connection between the pi i(13/2) circle times nu i(13/2) band and the ground-state band in Au-184 has been established, leading to a firm spin-and-parity assignment for the pi i(13/2) circle times nu i(13/2) band. The low-spin signature inversion is found in the pi i(13/2) circle times nu i(13/2) bands according to our spin-assignment and-the signature crossing observed at high-spin states.

A facile and effective method for the distribution of Mo/HZSM-5 catalyst active centers

Post-steaming treatment of Mo/HZSM-5 catalysts results in more molybdenum species migrating into and residing in the HZSM-5 zeolite channels. This is confirmed by XRF and XPS measurements. H-1 MAS NMR and Si-29 MAS NMR also demonstrate that the number of free Bronsted acid sites decreases in the Mo/HZSM-5 catalysts that underwent post-steaming treatment, compared to untreated Mo/HZSM-5 catalysts. As a result, the deactivation rate constant (kd) on the Mo/HZSM-5 catalyst after post-steaming treatment for 0.5 h is much smaller, and the catalyst therefore shows remarkable stability in the probe reaction of methane dehydro-aromatization. The results suggest that a more beneficial bi-functional balance between active Mo species for methane activation and acid sites for the following aromatization is developed over those Mo/HZSM-5 catalysts that have experienced post-steaming treatment for 0.5 h, in comparison with the untreated Mo/HZSM-5 catalysts.

Synthesis and Characterization of Urea Bridged Hybrid Periodic Mesoporous Organosilica Materials

Urea bridged organic-inorganic hybrid mesoporous SiO2 materials (U-BSQMs) were synthesized through a sol-gel procedure by co-condensation of bis(triethoxysilyl propyl) urea (BSPU) under basic conditions using cetyltrimethylammonium bromide (CTAB) as organic template. X-ray diffraction (XRD) and transmission electron microscopy (TEM) confirmed the mesoporous structure of the sample. Fourier-transform infrared spectroscopy (FT-IR), solid state CP-MAS NMR spectroscopy of Si-29 (Si-29, CP-MAS NMR) and C-13 (C-13 CP NMR) indicated that most of the Si-C bonds are unbroken during the synthesis process.

Synthesis, Spectroscopic Properties, and Stabilities of Ternary Europium Complex in SBA-15 and Periodic Mesoporous Organosilica: A Comparative Study

Ternary europium complex Eu(tta)(3)phen was covalently bonded with the general mesoporous. material SBA-15 and SBA-15-type of periodic mesoporous organosilica (PMO) material via impregnation of Eu(tta)(3)center dot 2H(2)O into phen-S15 and phen-PMO, respectively, through a ligand exchange reaction. The parent materials of phen-S15 and phen-PMO were synthesized by co-condensation of tetraethylorthosilicate (TEOS) or 1,2-bis(triethoxysilyl)ethane (BTESE) and the functionalized chelate ligand 5-(N,N-bis(3-triethoxysilyl)propyl)ureyl-1,10-phenanthroline (phen-Si) in the presence of Pluronic P123 surfactant as template, which were confirmed by SEM, XRD, FTIR, Si-29 CP-MAS NMR, and N-2 adsorption measurements.

Effect of silver nanoparticles on luminescent properties of europium complex in di-ureasil hybrid materials

Organic-inorganic hybrids containing luminescent lanthanide complex Eu(tta)(3)Phen (tta = thenoyltrifluoroaceton, phen = 1,10-phenanthroline) and silver nanoparticles have been prepared via mixing rare earth complex and nanoparticles with the precursors of di-ureasil using a sol-gel process. The obtained hybrid materials with transparent and elastomeric features were characterized by transmission electron microscope, solid-state Si-29 magic-angle spinning NMR spectra, diffuse reflectance, UV-visible absorption and photoluminescence spectroscopies. The effect of the silver nanoparticles on the luminescence properties was investigated. The experimental results showed that the luminescence intensity of the Eu(tta)(3)phen complex could be enhanced by less than ca. 9.5 nM of silver nanoparticles with the average diameter of 4 nm, and reached its maximum at the concentration of ca. 3.6 nM. Further increasing the concentration of the silver nanoparticles (> 9.5 nM) made the luminescence quenched. The enchancement and quench mechnism was discussed.

Surface-grafted silica linked with L-lactic acid oligomer: A novel nanofiller to improve the performance of biodegradable poly(L-lactide)

A new surface modification method by grafting L-lactic acid oligomer onto the surface silanol groups of silica nanoparticles has been developed. The surface-grafting reaction is confirmed by IR and Si-29 MAS NMR analyses. TEM and SEM results show that grafted SiO2 (g-SiO2) nanoparticles can be comparatively uniformly dispersed in chloroform or PLLA matrix, while the unmodified SiO2 nanoparticles tend to aggregate. The loading of g-SiO2 nanoparticles in poly(L-lactide) (PLLA) matrix greatly improves the toughness and tensile strength of this material. In contrast, the incorporation of un-grafted SiO2 nanoparticles into PLLA leads to the deterioration of its mechanical properties. DSC analysis shows that g-SiO2 nanoparticles can serve as a nucleating agent for the crystallization of PLLA in the composites. SEM characterization shows the tough characteristics and great interfacial combination strength for g-SiO2 (5wt%)/PLLA nanocomposites.

Novel acidic porous clay heterostructure with highly ordered organic-inorganic hybrid structure: one-pot synthesis of mesoporous organosilica in the galleries of clay

A new class of organic-inorganic hybrid porous clay heterostructures (HPCHs) have been prepared through the surfactant-directed assembly of organosilica in the galleries of montmorillonite. The reaction involved hydrolysis and condensation of phenyltriethoxysilane and tetraethoxysilane in the presence of intragallery surfactant templates (dodecylame and cetyltrimethylammonium ion). The surfactant templates were removed from the pores by solvent-extraction. The products were characterized by X-ray diffraction (XRD), N-2 adsorption, solid-state Si-29 and C-13 NMR, and FTIR. XRD patterns indicated a regular interstratification of the clay layers for HPCHs. Depending on loading of phenyl groups, HPCHs had BET surface areas of 390-771 m(2) g(-1), pore volumes of 0.3-0.59 cm(3) g(-1), and the framework pore sizes in the supermicropore to small mesopore range (1.2-2.6 nm). HPCHs were hydrophobic and acidic.

Stable ordered mesoporous silica materials templated by high-temperature stable surfactant micelle in alkaline media

Ordered hexagonal mesoporous silica material (JLU-30) has been successfully synthesized in alkaline media at high temperature (> 160 degreesC, using cationic (1,3-dimethyl-2-imidazolidin-2-ylidene)hexadecylmethyl-ammonium bromide (DIHAB) as a template, and characterized with X-ray diffraction (XRD), transmission electron microscopy (TEM), nitrogen adsorption-desorption isotherms, differential thermal analysis (DTA), and thermogravimetric analysis (TG), as well as Al-27 and Si-29 nuclear magnetic resonance (NMR) spectroscopy. Mesoporous JLU-30 shows much higher hydrothermal stability than MCM-41. Si-29 NMR spectra indicate that the pore walls of JLU-30 samples synthesized at high temperature (160 degreesC) are fully condensed, giving a Q(4)/Q(3) ratio as high as 6.2. In contrast, MCM-41 synthesized at relatively low temperature (100 degreesC) shows the Q(4)/Q(3) + Q(2) ratio at 1.1. Such unique structural feature might be responsible for the observed highly hydrothermal stability of the mesoporous silica materials (JLU-30).

Conductive polyaniline/silica hybrids from sol-gel process

A hybrid material with a conductive organic network in an inorganic matrix has been prepared by in-situ hydrolysis/polycondensation of TEOS in an aqueous solution of a solubilized polyaniline. Due to intense hydrogen bonding (indicated by Si-29 NMR and FTIR) the conductive polymer is very well dispersed in the silica matrix. The Figure shows SEM images of a 46/54 wt.-% hybrid at two temperatures (left 20 degreesC, right 100 degreesC).

High resolution solid-state NMR and DSC study of poly(ethylene glycol) silicate hybrid materials via sol-gel process

Hybrid materials incorporating poly(ethylene glycol) (PEG) with tetraethoxysilane (TEOS) via a sol-gel process were studied for a wide range of compositions of PEG by DSC and high resolution solid-state C-13- and Si-29-NMR spectroscopy. The results indicate that the microstructure of the hybrid materials and the crystallization behavior of PEG in hybrids strongly depend on the relative content of PEG. With an increasing content of PEG, the microstructure of hybrid materials changes a lot, from intimate mixing to macrophase separation. It is found that the glass transition temperatures (T-g) (around 373 K) of PEG homogeneously embedded in a silica network are much higher than that (about 223 K) of pure PEG and also much higher in melting temperatures T-m (around 323 K) than PEG crystallites in heterogeneous hybrids. Meanwhile, the lower the PEG content, the more perfect the silica network, and the higher the T-g of PEG embedded in hybrids. An extended-chain structure of PEG was supposed to be responsible for the unusually high T-g of PEG. Homogeneous PEG-TEOS hybrids on a molecular level can be obtained provided that the PEG. content in the hybrids is less than 30% by weight. (C) 1998 John Wiley & Sons, Inc.

MICROSTRUCTURE ANALYSIS OF 3 SEGMENTED COPOLYMERS CONTAINING POLYDIMETHYLSILOXANE BY SOLID-STATE HIGH-RESOLUTION NMR

The microstructure of two bicomponent and one tricomponent segmented copolymers, based on polydimethylsiloxane, poly(p-hydroxystyrene) or/and polysulfone, were investigated using an extended Goldman-Shen pulse sequence, proton spin-spin relaxation measurements, and C-13 and Si-29 NMR spectra. The results indicate that there exist four phases with different sizes, components and morphological structure in the segmented copolymers studied in this work, i. e., a rigid-chain phase of very slow motion, a rigid-chain-rich phase of slow motion, a flexible-chain-rich phase of fast motion and a flexible-chain phase of faster motion. The sizes of different domains, calculated from the spin diffusion rates, are about 50-100 angstrom for the flexible-chain-rich phase of fast motion and 200-300 angstrom for the flexible-chain phase of faster motion. The relative quantities of polydimethylsiloxane in the flexible-chain phase of fast motion are slightly different in different kinds of segmented copolymers.

晋北高岭石及其热产物的矿物物理学研究

通过对晋北地区高岭石及其热产物的研究，笔者主要得到了以下几点结论：1、晋北煤矸石是一种优质的高岭石，Fe、Ti含量低，结晶度高，晶体主要呈片状形态，具有较好的开发前景，应打破仅仅局限于陶瓷工业的局面。而P-1高岭石因Fe、Ti含量高，质量差。2、在高岭石受热脱羟过程中，部分羟基一直到850℃才完全脱失。3、在高岭石-莫来石反应系列中，存在SiO_2与Al_2O_3的分凝，SiO_2与Al_2O_3反应生成莫来石是莫来石的主要形成途径，Al-Si尖晶石与SiO_2反应生成莫来石只是一个次要途径。4、在高岭石热处理产物的研究中首次测到了-70ppm附近的Al-Si尖晶石的~(29)Si MAS NMR谱峰，Al-Si尖晶石是一个不稳定相，存在的温度范围大约为850-1000℃，随着温度升高，它将转变为莫来石。5、高岭石的980℃放热峰归因于在高岭石受热相变过程中，莫来石、方英石、γ-Al_2O_3的晶出。6、在煤矸石中，Fe主要以Fe~(2+)置换Al~(3+)形式存在，其次是部分Fe~(2+)被吸附在高岭石表面；而在P-1高岭石中，Fe主要以Fe~(3+)、Fe~(2+)置换Al~(3+)及杂质氧化物的形式存在。7、以前国内一些学者提出的所谓新矿物—“偏岭石”，笔者认为很可能是高岭石受煤自然烘烤形成的变高岭石。

NMR study on the acidity of TS-1 zeolite

The acidic properties of TS-1 and Silicalite-I zeolites have been investigated by the solid-state MAS NMR technique capable of in situ sample pretreatment. As shown by a combination of the P-31 MAS NMR and H-1 MAS NMR techniques with trimethylphosphine, not only Bronsted acid sites but also Lewis acid sites exist in the TS-1 zeolites. Moreover, TS-1 zeolite is more acidic compared with Silicalite-1. The H-1, Si-29 MAS NMR spectra and the resonance related to Bronsted acid species in the P-31 MAS NMR spectra demonstrate clearly that the presence of titanium in the framework results in the formation of a new hydroxy group, titanols, which is more acidic than silanols of Silicalite-1. The P-31 MAS NMR measurements also illustrate convincingly the existence of at least two different Lewis acid species on the TS-1 zeolites. The conversion of propylene oxide into methoxypropanol catalyzed by TS-1 or Silicalite-I zeolite in methanol solution as a test reaction has also been described. With the increase of titanium in zeolite, TS-1 appears to have a higher activity during the reaction of propylene oxide to methoxypropanol.