Pyrochlore structure La2Sn2O7:Eu3+ microcrystals with uniform octahedron shape were successfully synthesized via a hydrothermal route at 180 °C for 36 h. The crystal structure, particle size, morphologies, and ...Pyrochlore structure La2Sn2O7:Eu3+ microcrystals with uniform octahedron shape were successfully synthesized via a hydrothermal route at 180 °C for 36 h. The crystal structure, particle size, morphologies, and optical properties of the as-synthesized products were investigated by XRD, TEM, SEM, EDS, FT-IR, Raman spectroscopy and PL. The effects of pH of precursor solution, precursor concentration, reaction temperature, and time were investigated. The results reveal that pH of the precursor solution not only plays an important role in determining the phase of the as-synthesized products, but also has a significant influence on the morphologies of the samples. High-quality and uniform octahedrons with an average size of about 700 nm could be easily obtained at the pH value of 12. The possible formation mechanism of octahedral-like La2Sn2O7:Eu3+ microcrystals was briefly proposed. The photoluminescence spectra show that La2Sn2O7:Eu3+ micro-octahedra display stronger emission in the range of 582-592 nm compared with the samples with other shapes.展开更多
Among the reactions catalyzed by zeolites there are some that exhibit high selectivity due to the spatial confinement effect of the zeolite framework.Tailoring the acidity,particularly the distribution and location of...Among the reactions catalyzed by zeolites there are some that exhibit high selectivity due to the spatial confinement effect of the zeolite framework.Tailoring the acidity,particularly the distribution and location of the Bronsted acid sites in the zeolite is effective for making it a better catalyst for these reactions.We prepared a series of H-mordenite(H-MOR) samples by varying the composition of the sol-gel,using different structure directing agents and post-treatment.NH3-TPD and IR characterization of adsorbed pyridine were employed to determine the amount of Bronsted acid sites in the 8-membered ring and 12-membered ring channels.It was shown that controlled synthesis was a promising approach to improve the concentration of Bronsted acid sites in MOR,even with a low Al content.Using an appropriate composition of Si and Al in the sol-gel favored a higher proportion of Bronsted acid sites in the 8-membered ring channels.HMI as a structure-direct agent gave an obvious enrichment of Bronsted acid sites in the 8-membered ring.Carbonylation of dimethyl ether was used as a probe reaction to examine the modification of the acid properties,especially the Bronsted acid sites in the 8-membered ring channels.There was a linear relationship between methyl acetate formation and the number of Bronsted acid sites in the 8-membered ring channels,demonstrating the successful modification of acid properties.Our results provide information for the rational design and modification of zeolites with spatial constraints.展开更多
(E) -4-chloro-4' -ethoxystilbene (2a) and (E) -4, 4' - dichlorostilbene (2b) were synthesized by the Witting-Homer reaction. The crystals of 2a and 2b were prepared through solvent evaporation and characteri...(E) -4-chloro-4' -ethoxystilbene (2a) and (E) -4, 4' - dichlorostilbene (2b) were synthesized by the Witting-Homer reaction. The crystals of 2a and 2b were prepared through solvent evaporation and characterized by the single-crystal X- ray diffraction. Molecular structure analysis confirms the E- configuration of C=C bond. The crystal of 2a reveals an orthorhombic and space group Pna21 structure while 2b shows a monoclinic and space group P21/c structure. The electronic structures of 2a and 2b were optimized at B3LYP/6-311 + + G (d, p) level. The Hirshfeld surface and fingerprint plot indicate close O-H and C1-H contacts and π-π stacking in 2a and 2b. Molecular electrostatic potential shows that the O and C1 atoms of 2a and C1 atoms of 2b have the minimum energies and they are more likely to be attacked by electrophiles in reaction. Frontier molecular orbitals analysis demonstrates that the △ELuMO_HOMO of 2a and 2b are 3.85 and 3.91 eV, respectively.展开更多
Highly efficient synthesis methods have been developed and characteristics of nanometallocarbosilanes molecular structure were studied by the research team of GNIIChTEOS (State Research Institute for Chemistry and Te...Highly efficient synthesis methods have been developed and characteristics of nanometallocarbosilanes molecular structure were studied by the research team of GNIIChTEOS (State Research Institute for Chemistry and Technology of Organoelement Compounds). Nanometallocarbosilanes were synthesized by thermal co-condensation of oligocarbosilanes and alkyl amides of refractory metals. Initial, intermediate and final products of side reactions were characterized by 1H, 13C, 29Si NMR (nuclear magnetic resonance), IR (infra-red) spectroscopy, GPC (gel-penetrating chromatography), TGA (thermal gravimetric analysis), TEM (transmission electron microscopy), SEM (scanning electron microscopy), RES (X-ray phase analysis) and elemental analysis. The proposed synthesis method of nanometallocarbosilanes was lbund to produce fusable soluble organosilicon oligomers with homogeneous distribution of nanoscale (10-20 nm) metal particles in the oligomer matrix. A computational model of the group and elemental composition of nanometallocarbosilanes was developed; it was shown that they are molecular globules of near-spherical shape and rigid polycyclic structure. Thermochemical treatment of nanometallocarbosilanes leads to SiC-nanoceramics (a high yield of up to 75-80 mass%) modified by metal nanoparticles (20-30 nm) contributing to its stabilization. The application of preceramic oxygen-free nanometallocarbosilanes will make it possible to advance in solving the problem of ceramic composite materials with long-term resistance at temperatures above 1,500 ℃ in oxidizing environments.展开更多
The Ti Bw reinforced near-α titanium matrix composite(Ti-5.8 Al-3.4 Zr-4.0 Sn-0.4 Mo-0.4 Nb-0.4 Si-0.06 C) was successfully synthesized by powder metallurgy and hot extrusion route. The effects of solution and agin...The Ti Bw reinforced near-α titanium matrix composite(Ti-5.8 Al-3.4 Zr-4.0 Sn-0.4 Mo-0.4 Nb-0.4 Si-0.06 C) was successfully synthesized by powder metallurgy and hot extrusion route. The effects of solution and aging temperature on the microstructure and high temperature tensile properties of the composite were investigated. The results revealed that the fine transformed β phase can be obtained by the solution treatment at β phase region and aging treatment, no other precipitates were observed. The α2 phase(Ti3 Al) can be acquired when the solution treated at α+β phase region followed by aging treatment. With increasing the aging temperature from 500 to 700℃ for 5 h, the size of α2 precipitates increases from about 5 to about 30 nm. The Ti Bw are stable without any interfacial reaction during the heat treatments. The high temperature tensile properties show that the composite performed by solution and aging treatment exhibits good strengthening effects. With increasing the aging temperature from 500 to 700℃, the strength of the composite increases at the expense of elongation due to the increment of α2 precipitates.The strength of the composite at 600℃ increases by 17% to 986 MPa after 1000℃/2 h/AC and 700℃/5 h/AC heat treatment.展开更多
基金Project (07C26214301746) supported by Innovation Foundation of Ministry of Science and Technology, ChinaProject (2010GXNSFB013008) supported by Guangxi Natural Science Foundation, ChinaProject (2009bsxt001) supported by the Graduate Degree Thesis Innovation Foundation of Central South University, China
文摘Pyrochlore structure La2Sn2O7:Eu3+ microcrystals with uniform octahedron shape were successfully synthesized via a hydrothermal route at 180 °C for 36 h. The crystal structure, particle size, morphologies, and optical properties of the as-synthesized products were investigated by XRD, TEM, SEM, EDS, FT-IR, Raman spectroscopy and PL. The effects of pH of precursor solution, precursor concentration, reaction temperature, and time were investigated. The results reveal that pH of the precursor solution not only plays an important role in determining the phase of the as-synthesized products, but also has a significant influence on the morphologies of the samples. High-quality and uniform octahedrons with an average size of about 700 nm could be easily obtained at the pH value of 12. The possible formation mechanism of octahedral-like La2Sn2O7:Eu3+ microcrystals was briefly proposed. The photoluminescence spectra show that La2Sn2O7:Eu3+ micro-octahedra display stronger emission in the range of 582-592 nm compared with the samples with other shapes.
基金supported by the National Natural Science Foundation of China(21325626,21406120)the Postdoctoral Science Foundation of China(2014M560181,2015T80214)~~
文摘Among the reactions catalyzed by zeolites there are some that exhibit high selectivity due to the spatial confinement effect of the zeolite framework.Tailoring the acidity,particularly the distribution and location of the Bronsted acid sites in the zeolite is effective for making it a better catalyst for these reactions.We prepared a series of H-mordenite(H-MOR) samples by varying the composition of the sol-gel,using different structure directing agents and post-treatment.NH3-TPD and IR characterization of adsorbed pyridine were employed to determine the amount of Bronsted acid sites in the 8-membered ring and 12-membered ring channels.It was shown that controlled synthesis was a promising approach to improve the concentration of Bronsted acid sites in MOR,even with a low Al content.Using an appropriate composition of Si and Al in the sol-gel favored a higher proportion of Bronsted acid sites in the 8-membered ring channels.HMI as a structure-direct agent gave an obvious enrichment of Bronsted acid sites in the 8-membered ring.Carbonylation of dimethyl ether was used as a probe reaction to examine the modification of the acid properties,especially the Bronsted acid sites in the 8-membered ring channels.There was a linear relationship between methyl acetate formation and the number of Bronsted acid sites in the 8-membered ring channels,demonstrating the successful modification of acid properties.Our results provide information for the rational design and modification of zeolites with spatial constraints.
文摘(E) -4-chloro-4' -ethoxystilbene (2a) and (E) -4, 4' - dichlorostilbene (2b) were synthesized by the Witting-Homer reaction. The crystals of 2a and 2b were prepared through solvent evaporation and characterized by the single-crystal X- ray diffraction. Molecular structure analysis confirms the E- configuration of C=C bond. The crystal of 2a reveals an orthorhombic and space group Pna21 structure while 2b shows a monoclinic and space group P21/c structure. The electronic structures of 2a and 2b were optimized at B3LYP/6-311 + + G (d, p) level. The Hirshfeld surface and fingerprint plot indicate close O-H and C1-H contacts and π-π stacking in 2a and 2b. Molecular electrostatic potential shows that the O and C1 atoms of 2a and C1 atoms of 2b have the minimum energies and they are more likely to be attacked by electrophiles in reaction. Frontier molecular orbitals analysis demonstrates that the △ELuMO_HOMO of 2a and 2b are 3.85 and 3.91 eV, respectively.
文摘Highly efficient synthesis methods have been developed and characteristics of nanometallocarbosilanes molecular structure were studied by the research team of GNIIChTEOS (State Research Institute for Chemistry and Technology of Organoelement Compounds). Nanometallocarbosilanes were synthesized by thermal co-condensation of oligocarbosilanes and alkyl amides of refractory metals. Initial, intermediate and final products of side reactions were characterized by 1H, 13C, 29Si NMR (nuclear magnetic resonance), IR (infra-red) spectroscopy, GPC (gel-penetrating chromatography), TGA (thermal gravimetric analysis), TEM (transmission electron microscopy), SEM (scanning electron microscopy), RES (X-ray phase analysis) and elemental analysis. The proposed synthesis method of nanometallocarbosilanes was lbund to produce fusable soluble organosilicon oligomers with homogeneous distribution of nanoscale (10-20 nm) metal particles in the oligomer matrix. A computational model of the group and elemental composition of nanometallocarbosilanes was developed; it was shown that they are molecular globules of near-spherical shape and rigid polycyclic structure. Thermochemical treatment of nanometallocarbosilanes leads to SiC-nanoceramics (a high yield of up to 75-80 mass%) modified by metal nanoparticles (20-30 nm) contributing to its stabilization. The application of preceramic oxygen-free nanometallocarbosilanes will make it possible to advance in solving the problem of ceramic composite materials with long-term resistance at temperatures above 1,500 ℃ in oxidizing environments.
基金supported by the National Natural Science Foundation of China(Grant Nos.51701114,11604204,51471063,51271111)the Youth Teacher Development Program of Shanghai Universities(Grant No.ZZGCD15101)+1 种基金Scientific Research Project of Shanghai University of Engineering ScienceTalents Project of Shanghai University of Engineering Science
文摘The Ti Bw reinforced near-α titanium matrix composite(Ti-5.8 Al-3.4 Zr-4.0 Sn-0.4 Mo-0.4 Nb-0.4 Si-0.06 C) was successfully synthesized by powder metallurgy and hot extrusion route. The effects of solution and aging temperature on the microstructure and high temperature tensile properties of the composite were investigated. The results revealed that the fine transformed β phase can be obtained by the solution treatment at β phase region and aging treatment, no other precipitates were observed. The α2 phase(Ti3 Al) can be acquired when the solution treated at α+β phase region followed by aging treatment. With increasing the aging temperature from 500 to 700℃ for 5 h, the size of α2 precipitates increases from about 5 to about 30 nm. The Ti Bw are stable without any interfacial reaction during the heat treatments. The high temperature tensile properties show that the composite performed by solution and aging treatment exhibits good strengthening effects. With increasing the aging temperature from 500 to 700℃, the strength of the composite increases at the expense of elongation due to the increment of α2 precipitates.The strength of the composite at 600℃ increases by 17% to 986 MPa after 1000℃/2 h/AC and 700℃/5 h/AC heat treatment.