Research Progress of Carbon-Silicone Composite Materials

Silicone is a kind of polymer material with high cross-linked structure,which is com-posed by Si-O-Si main chain.Due to the special molecular chain structure,silicone mate-rials are characterized by oxidation resistance,aging resistance,high and low temperature resistance and chemical corrosion resistance.Moreover,silicone materials have process-able properties,simple forming process,good mechanical property,non-toxic and pollution-free.Therefore,silicone has been widely concerned by researchers at home and abroad.In this paper,the main research progress and application directions of carbon-silicone composite at home and abroad in recent years are reviewed.

Upconversion luminescence of Y_2O_3:Er^(3+), Yb^(3+) nanoparticles prepared by a homogeneous precipitation method

Y2O3： Er^3＋, Yb^3＋ nanoparticles were synthesized by a homogeneous precipitation method without and with different concentrations of EDTA 2Na. Upconversion luminescence spectra of the samples were studied under 980 nm laser excitation. The results of XRD showed that the obtained Y2O3：Er^3＋,Yb^3＋ nanoparticles were of a cubic structure. The average crystallite sizes calculated were in the range of 28-40 nm. Green and red upconversion emission were observed, and attributed to ^2H11/2,^4S3/2→^4I15/2 and ^4F9/2→^4I15/2 transitions of the ion, respectively. The ratio of the intensity of green emission to that of red emission drastically changed with a change in the EDTA 2Na concentration. In the sample synthesized without EDTA, the relative intensity of the green emission was weaker than that of the red emission. The relative intensities of green emission increased with the increased amount of EDTA 2Na used. The possible upconversion luminescence mechanisms were discussed.

Biodegradation of 2-naphthol and its metabolites by coupling Aspergillus niger with Bacillus subtilis

To explore biodegradation of 2-naphthol and its metabolites accumulated in wastewater treatment,a series of bio-degradation experiments were conducted.Two main metabolites of 2-naphthol,1,2-naphthalene-diol and 1,2-naphthoquinone,were identified by high-performance liquid chromatography with standards.Combining fungus Aspergillus niger with bacterium Bacillus subtilis in the treatment enhanced 2-naphthol degradation efficiency,lowered the accumulation of the two toxic metabolites.There were two main phases during the degradation process by the kinetic analysis：2-naphthol was first partly degraded by the fungus,producing labile and easily accumulated metabolites,and then the metabolites were mainly degraded by the bacterium,attested by the degradation processes of 1,2-naphthalene-diol and 1,2-naphthoquinone as sole source of carbon and energy.Sodium succinate,as a co-metabolic substrate,was the most suitable compound for the continuous degradation.The optimum concentration of 2-naphthol was 50 mg/L.The overall 2-naphthol degradation rate was 92%,and the COD Cr removal rate was 80% on day 10.These results indicated that high degradation rate of 2-naphthol should not be considered as the sole desirable criterion for the bioremediation of 2-naphtholcontaminated soils/wastewater.

Degradation of metabolites of benzo[a]pyrene by coupling Penicillium chrysogenum with KMnO_4

Several main metabolites of benzo[a]pyrene （BaP） formed by Penicillium chrysogenum, Benzo[a]pyrene-1,6-quinone （BP 1,6- quinone）, trans-7,8-dihydroxy-7,8-dihydrobenzo[a]pyrene （BP 7,8-diol）, 3-hydroxybenzo[a]pyrene （3-OHBP）, were identified by high-performance liquid chromatography （HPLC）. The three metabolites were liable to be accumulated and were hardly further metabolized because of their toxicity to microorganisms. However, their further degradation was essential for the complete degradation of BaP. To enhance their degradation, two methods, degradation by coupling Penicillium chrysogenum with KMnO4 and degradation only by Penicillium chrysogenum, were compared; Meanwhile, the parameters of degradation in the superior method were optimized. The results showed that （1） the method of coupling Penicillium chrysogenum with KMnO4 was better and was the first method to be used in the degradation of BaP and its metabolites; （2） the metabolite, BP 1,6-quinone was the most liable to be accumulated in pure cultures; （3） the effect of degradation was the best when the concentration of KMnO4 in the cultures was 0.01% （w/v）, concentration of the three compounds was 5 mg/L and pH was 6.2. Based on the experimental results, a novel concept with regard to the bioremediation of BaP-contaminated environment was discussed, considering the influence on environmental toxicity of the accumulated metabolites.

Synthesis of Vanadium Nitride by a One Step Method

Vanadium nitrides were prepared via one step method of carbothermal reduction and nitridation of vanadium trioxide. Thermalgravimetric analysis （TGA） and X-ray diffraction were used to determine the reaction paths of vanadium carbide, namely the following sequential reaction： V2O3→V8C7 in higher temperature stage, the rule of vanadium nitride synthesized was established, and defined conditions of temperature for the production of the carbides and nitrides were determined. Vanadium oxycarbide may consist in the front process of carbothermal reduction of vanadium trioxide. In one step method for vanadium nitride by carbothermal reduction and nitridation of vanadium trioxide, the nitridation process is simultaneous with the carbothermal reduction. A one-step mechanism of the carbothermal reduction with simultaneous nitridation leaded to a lower terminal temperature in nitridation process for vanadium nitride produced, compared with that of carbothermal reduction process without nitridation. The grain size and shape of vanadium nitride were uniform, and had the shape of a cube. The one step method combined vacuum carborization and nitridation （namely two step method） into one process. It simplified the technological process and decreased the costs.

Synthesis and Anti-tumor Activity of Novel Amide Derivatives of Ursolic Acid

Ursolic acid was modified at C3 and C28 position to obtain fourteen derivatives including twelve novel compounds, and their chemical structures were characterized by IR, ^1H NMR and MS. Cell growth inhibitory effects of the derivatives against Hela cell were evaluated by MTT assay. All these derivatives were found to have stronger cell growth inhibitory than their parent compound, ursolic acid. The derivatives with a substituted acetyl group at C3 hydroxyl group show better activities than those with an unsubstituted hydroxyl group.

Efficiency of Plate Separators for Dispersed Liquid-Liquid Systems

The basic flow model of laminar flow field and the trajectory model of dispersed phase drops are derived. Based on the comparable volumetric flow rate, the dispersed flow rate can be linearly discretized. Consequently, the trajectory of a droplet in the channel can be tracked, and the trajectories of all drops are observed in order to statistically analyse the drops for capture or entrainment. Therefore,in terms of theoretical model of motion,the stratified two phase flow systems are studied in the mixture of nitrobenzene and concentrated sulfuric acid. The analytical results indicate that the trajectories of droplets of different diameters are different at the same location. The larger droplets can help to promote the efficiency of plate separators. The thickness of trickling film has a significant influence on the efficiency of numerical simulation when the concentration of the dispersed phase is greater than 100/0. So the modification of thickness of trickling film can help to get the real flow field efficiency. The low flow rate lowers the average Renolds number so that the lighter phase droplets have sufficient time to interact with the trickling film. It is an indispensable factor for predicting efficiency that coalesced drops flow off inclined plates together with trickling films. A comparison confirms that the simulation results are in good agreement with the experiment results.

Synthesis of Long Afterglow Photoluminescent Materials Sr_2MgSi_2O_7∶Eu^(2+), Dy^(3+) by Sol-Gel Method

Long afterglow photoluminescent materials Sr2MgSi2O7 doped with Eu2+, Dy3+ were prepared by sol-gel method. The synthesized samples were characterized by X-ray diffraction. The excitation spectrum, emission spectrum and long decay curve were measured and analyzed. XRD pattern indicates that phosphor is with Sr2MgSi2O7 crystal structure. The wide range of excitation wavelength indicates that luminescent material can be excited by light from ultraviolet ray to visible light. The main peak of emission spectrum is located at 466 nm. Sample excited by visible light can emit bright blue light, and the afterglow time lasts more than 8 h.

Effect of Yb^(3+) concentration on the structures and upconversion luminescence properties of Y_2O_3:Er^(3+) ultrafine phosphors

Y2O3：Er^3＋ ultrafine phosphors with a varying Yb^3＋ ion concentration were prepared by a urea homogeneous precipitation method. The results of XRD show that all the samples are of a pure cubic structure and the average crystallite sizes can be calculated as 45, 34, and 28 nm for Y2O3：Er^3＋ ultrafine phosphors with Yb^3＋ ion concentrations of 0, 10%, and 20%, respectively. The lattice constant and cell volume of the ultrafine phosphors decrease with enhancing Yb^3＋ ion concentration. The upconversion luminescence spectra of all the samples were studied under 980 nm laser excitation. The strong green and red upconversion emission were observed, and attributed to the ^2H11/2→^4I15/2, ^4S3/2 → ^4I15/2 and ^4F9/2 →^4I15/2 transitions of Er^3＋, respectively. The intensity of red emission increases with increasing Yb^3＋ ion concentration. The effect of Yb^3＋ ion concentration on the structures and upconversion luminescence mechanism were discussed.

Synthesis and Crystal Structure of a Two-dimensional Framework Supramolecular Complex [Mn(phen)(DPZDA)(H_2O)]·2H_2O

A novel two-dimensional supramolecular complex [Mn（phen）（DPZDA）（H2O）]·2H2O has been synthesized by the reaction of Mn（CH3COO）2, 1,10-phenanthroline （phen） and H2DPZDA （3,5-dimethyl-pyrazine-2,6-dicarboxylic acid）. Elemental analysis, IR spectra and X-ray singlecrystal diffraction were carried out to determine the composition and crystal structure of the title complex. Crystal data： triclinic system, space group P1, a = 7.7474（13）, b = 9.3381（15）, c = 15.146（3） A, α = 93.872（3）, β= 102.451 （11 ）, y = 105.261 （ 11）°, C20H20MnN4O7, Mr = 483.34, Z = 2, F（000） = 498, V=1023.2（3）A^3, Dc=1.569 g/cm^3,μ=0.697 mm^-1, -9≤h≤9, -11≤k≤10, -18≤l≤12, R = 0.0365 and wR=0.0901 for 3585 independent reflections （Rint= 0.0165） and 2923 observed reflections （I〉 2σ（I））. Structural analysis indicates that Mn（Ⅱ） adopts a distorted octahedral geometry. The 2-D framework supramolecular structure of the title complex is constructed from hydrogen bonds and π…π interactions.

Synthesis and Crystal Structure of a Ternary Complex:[Ni(phen)_2(pmal)]·8H_2O

A new ternary complex [Ni（phen）（pmal）]·8H2O （phen = 1,10-phenanthroline, pmal^2- = phenethyl malonic acid） has been synthesized by the reaction of nickel acetate, phen and phenethyl malonic acid. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. Crystal data for this complex： triclinic system, space group PI^-, a = 10.387（5）, b = 13.112（6）, c = 14.229（6） °A, α= 76.176（7）, β = 83.778（8）, γ = 71.770（6）°, C35H42N4O12Ni, Mr= 769.44, Z = 2, F（000） = 808, V = 1786.1°A^3, Dc = 1.431 g/cm^3,μ= 0.612 mm^-1, the final R = 0.0653 and wR = 0.1033 for 9379 （Rint = 0.0244） independent reflections and 4730 observed reflections （I〉 2σ（I））. Structural analysis shows that the coordination geometry of Ni（Ⅱ） is a distorted octahedron. A novel two-dimensional structure is constructed from （H2O）4 and （H2O）12 water clusters, and the complex forms a 3-D network supramolecular structure by hydrogen bonds and π-π stacking of neighboring phens.

Synthesis and Crystal Structure of Complex [Pb(qina)_2(DMSO)]·H_2O

A novel complex [Pb（qina）2（DMSO）]·H2O was synthesized, of which qinais the quinaldic acid radical and DMSO the dimethyl sulfoxide. Elemental analysis, IR spectra, and X-ray single-crystal diffraction were carried out to determine the composition and crystal structure. This complex belongs to monoclinic system, space group P121/n1, with a = 7.1553（17）, b = 17.543（2）, c = 17.306（2） A, β = 91.671（4）°, C22H20N206PbS, Mr = 647.65, Z = 4, V= 2171.5（6） A3, Dc= 1.981 g/cm^3, μ= 7.908 mm^-1, F（000） = 1248, -9≤h≤6, -23≤k≤19, -22≤1≤22, R= 0.0221 and wR= 0.0488. Weak coordinate bond is formed between oxygen atom in DMSO and Pb（ Ⅱ ）. There are also weak interactions, such as π-π interaction, hydrogen bonds and so on, among the complex molecules.

Synthesis of Long Afterglow Phosphors MAl_2O_4∶Eu^(2+), Dy~ (3+)(M=Ca, Sr, Ba) by Microemulsion Method and Their Luminescent Properties

Long afterglow phosphors MAl2O4：Eu^2＋ , Dy^3＋ （M = Ca, Sr, Ba） were synthesized by microemulsion method, and their crystal structure and luminescent properties were compared and investigated. XRD patterns of samples indicate that phosphors CaAl2O4：Eu^2＋, Dy^3＋ and SrAl2O4 ： Eu^2＋, Dy^3＋ are with monoelinie crystal structure and phosphor BaAl2O4：Eu^2＋ , Dy^3＋ is with hexagonal crystal structure. The wide range of excitation spectrum of phosphors MAl2O4： Eu^2 ＋ , Dy^3＋ （M = Ca,Sr, Ba） indicates that the luminescent materials can he excited by light from ultraviolet ray to visible light and the maximum emission wavelength of phosphors MAl2O4：Eu^2＋ , Dy^3＋ （M = Ca, Sr, Ba） is found mainly at λem of 440 nm （M = Ca）, 520 nm （M = Sr） and 496 nm （M = Ba） respectively, the corresponding colors of emission light are blue, green and eyna-green respectively. The afterglow decay tendency of phosphors can he summarized as three processes： initial rapid decay, intermediate transitional decay and very long slow decay. Afterglow decay curves coincide with formula I = At^ - n, and the sequence of afterglow intensity and time is Sr 〉 Ca 〉 Ba.

Synthesis and Crystal Structure of the Binuclear Complex:[Cu_2(phen)_2(ip)(Hip)_2]·4H_2O

A binuclear complex [Cu2（phen）2（ip）（Hip）2].4H2O has been synthesized by the reaction of Cu（CH3COO）2.H2O, phen（1,10-phenanthroline） and isophthalic acid （H2ip） under hydrothermal condition. Elemental analysis, IR spectra and X-ray single-crystal diffraction were carded out to determine the composition and crystal structure. Crystal data for this complex： monoclinic, space group C2/c, a = 19.214（3）, b = 10.6973（14）, c = 22.567（3） A, β = 105.081（2）°, C24H19N2O8Cu, Mr= 526.95, Z = 8, F（000） = 2160, V= 4478.6（10） A3, Dc = 1.563 g/cm^3,μ = 1.030 mm^-1, -24≤h≤ 16, -13≤k≤13, -28≤l≤28, R = 0.0369 and wR = 0.0819 for 4615 （Rint = 1.0357） independent reflections and 3290 observed ones （I 〉 2σ（I））. Structural analysis shows that coordination geometry of Cu（ Ⅱ ） is a planar square, and the title complex exhibits a 2-D framework supramolecular structure by hydrogen bonds and π-π stacking interactions.

Synthesis and Crystal Structure of a 2D Coordination Polymer:[Nd_2(PDB)_2(CH_3COO)_2(H_2O)_3]

A novel coordination polymer [Nd2（PDB）2（CH3COO）2（H2O）3] （H2PDB = pyridine3,4-dicarboxylic acid） has been synthesized by the reaction of Nd（CH3COO）3 with pyridine3,4-dicarboxylic acid under hydrothermal conditions. Elemental analysis, IR spectra and X-ray crystal structure analysis were carried out to determine the composition and crystal structure of the title complex which belongs to the triclinic system, space group P^-1 with a = 6.9409（14）, b = 7.5497（15）, c = 22.530（5）A, α = 84.79（3）, β = 88.15（3）, γ= 75.55（3）^o, C18H18N2O15Nd2, Mr = 790.82, Z = 2, V = 1138.5（4） A^3, Dc = 2.307 g/cm^3,μ = 4.593 mm^-1, -6≤h≤8, -5≤k ≤8, -26≤l≤ 26, F（000） = 760, Rint = 0.0298, R= 0.0314 and wR= 0.0695 （I〉 2σ（I））. Nd（1） and Nd（2） are linked into zigzag chains by carboxylate groups of acetate with interesting μ3-η^2：η^2 fashion. The zigzag chains are bridged by PDB to form a 2D framework, and a 3D supramolecular network is further constructed via π-π stacking.

INVESTIGATION ON STABILITY OF PZT/EPOXY PIEZOCOMPOSITE WITH PRESSURE AND TEMPERATURE

With the universal test machine and temperature test chamber, the effect of pressure and temperature on the behavior of 1-3 and 1-3-2 piezocomposites prepared with PZT/epoxy in our lab has been investigated through electrical impedance and dielectric analysis. The permittivity, resonant frequency and dielectric loss of the composites have been measured under vertical stress and temperature, and the variety of the material properties under pressure and temperature could also be obtained. The pressure and temperature stability of the composites have been assessed through experiments. The data of these two types of composites indicated that the stability of 1-342 composite with pressure was better than that of 1-3 composite, and two composites have almost the same dielectric stability with temperature. However, 1-3-2 composite showed slower frequency variation than 1-3 composite.

Study on crystallization and microstructure of Li_2O-Al_2O_3-SiO_2 glass ceramics

Lithium aluminosilicate （LAS） glasses are generally difficult to prepare because of their high melting temperature. In this study, the preparation of LAS glasses was achieved at a relatively low melting temperature. The batch containing MgO-ZnO-LiEO- Al2O3-SiO2 was melted in a platinum crucible at 1550℃ for 2 h and was then followed by two- or three-step heat treatment processes for nucleation and crystal growth. The characterizations were carried out by differential thermal analysis, X-ray diffraction, infrared spectroscopy, scanning electron microscopy, and UV-Vis-NIR scanning spectrophotometry. The hexagonal stuffed β-eucryptite solid solution crystallized at 840-960℃. Most of the hexagonal β-eucryptite solid solution transformed into the tetragonal β-spodumene solid solution at 1100℃. Almost all the aluminum atoms entered into the tetrahedral sites in the aluminosilicate network of the 6- eucryptite/β-quartz solid solution. All of the Al atoms did not belong to the aluminosilicate network of the β-spodumene solid solution. The glass ceramic with a mean grain size of 10-20 nm is transparent, the transmittance reaches -85% in the visible light wavelength.

Effects of SiC and MgO on alumina-based ceramic foams filters

Alumina-based foam ceramic filters were fabricated by using alumina,SiC,magnesia powder as major materials.It has been found that this ceramic filter has a uniform macrostructure for filtering molten metals.The influences of SiC and magnesia content,the sintering temperatures on ceramic properties were discussed.Alumina-based foam ceramic filters containing 2.2 mass% magnesia and 7.6 mass% SiC has a compressive strength of 1.36 MPa and a thermal shock resistance of 5 times.Its main phases after 1 hour sintering at 1 500℃ consist of alumina,silicon carbide,spinel and mullite.

Synthesis,Structure and Properties of Three-dimensional Gd(Ⅲ),Eu(Ⅲ) Coordination Polymers via in situ Decarboxylation

Two three-dimensional lanthanide（Ⅲ） coordination polymers with the formula [Ln（PYDC）（NA）（H2O）]n [Ln=Gd（1）, Eu（2）, H2PYDC=pyridine-2,5-bicarboxylic acid, HNA=nicotinic acid] have been hydrothermally synthesized and characterized by elemental analysis, IR, and single crystal X-ray diffraction. The NA came from in situ decarboxylation of the part of PYDC. X-ray single crystal structural analyses reveal that complexes 1 and 2 are isomorphous, they possess the 43.63 topology assembled by Gd^3＋/Eu^3＋ and two different multidentate carboxylate ligands Magnetic measurements show that antiferromagnetic coupling exists between adjacent Gd^3＋ ions in complex 1. The complex 2 exhibits the corresponding characteristic luminescence in the visible region under an excitation at 305 nm.