水热法制备氧化镁／石墨烯复合材料的研究

以七水合硫酸镁（MgSO4·7H2O）和二水合碳酸铵（（NH4）2CO3·2H2O）为原料、聚乙烯吡咯烷酮（PVP）为分散剂,采用水热法制备了纳米氧化镁及其与石墨烯的复合材料,利用X射线衍射仪（XRD）和扫描电子显微镜（SEM）对样品进行了表征。结果表明,含10％石墨烯的复合材料中的MgO形状规则、颗粒较小、结晶性好、结晶度高。     

Syntheses and lyotropic liquid crystal properties of a series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30

A series of sandwich-type tungstoarsenates heteropoly compounds with As/W ratio of 4/30, Na16[As4W30M4(H2O)2O112]·XH2O (M = Zn,Cu,Co,Ni,Mn and Cd), have been synthesized for the first time and structurally characterized by elemental analysis, IR and 183W NMR spectra. The crystal structure of Na16[As4W30Cu4(H2O)2O112]·63H2O was determined to be a triclinic system, of P1 symmetry, a = 1.2721(3) nm, b = 2.451 6(5) nm, c = 2.6450(5) nm, α= 89.90(3)°,β= 77.32(3)°, γ= 89.96(3)°, 2=2. Using tetrahepty lammonium bromide as a phase transfer reagent, [As4W30Cu4(H2O)2O112]16- was transferred from aqueous solution to organic phase (benzene), and the heteropolyanion lost the coordination water molecules to form the coordination-unsaturated ion. After lactic acid was added to the benzene solution, the coordination-saturation was recovered. By esterification reaction between lactic acid and cholesterin, the latter was attached to the heteropolyanion indirectly. Therefore, a new type of lyotropic liquid crystal was obtained, which was characterized by a polarimicroscope, DSC and variable temperature wide-angle X-ray diffraction.     

Glass melt inclusion in clinopyroxene from Linqu Cenozoic basalt, Shandong Province, China

Melt inclusions or glasses usually occur in spinel- facies peridotitic xenoliths entrained in the global ba- salts[1―4], and olivine phenocrysts and/or xenocrysts carried in the intermediate-mafic volcanic rocks (such as basalts, basaltic andesites and h…     

Precipitation variability in central Himalayas and its relation to Northern Hemisphere temperature

Agriculture, industry and hydroelectric power in south Asia are heavily dependent on the performance of the summer (June to September) monsoon rainfall, which provides 75—90% of the annual rainwater over most parts of the area. A weak monsoon year generally corresponds to low crop yields. And strong monsoon usually produces abundant crops, although too much rainfall may produce devastating floods. However, modeling efforts to forecast the monsoon have met with only moderate success[1]. Prev…     

Magma mixing in upper mantle: Evidence from high Mg<Superscript>#</Superscript> olivine hosted melt inclusions in MORBs near East Pacific Rise 13°N

Early formed high-Mg^# olivine phenocrysts during evolution of MORB magmas usually host melt inclusions, which record im-portant information about the early-stage evolution of magma. Five MORB samples from near East Pacific Rise (EPR) 13°N vary little in K/Ti (0.07–0.12), Tb/Lu (1.72–1.84) and Sm/Nd (0.310–0.332) and have similar REEs patterns, indicating that depleted upper mantle has similar mineral composition. Sixty-five initial melt inclusions derived by correcting olivine fractionation and “FeO-Loss” show averagely higher MgO contents than their host rocks. Melt inclusions have higher CaO/Al₂O₃ ratios than their host rocks, and these CaO/Al₂O₃ ratios are positively and negatively correlated with MgO and Na₂O respectively, suggesting that these magmas have experienced high pressure crystallization of clinopyroxene. Average crystallization pressure, which is calculated based on the pressure dependence of clinopyroxene crystallization, is 0.83–0.25 GPa, and implys that these melt inclusions are averagely trapped in mantle depth of ~24 km. These melt inclusions show negative correlations of Ca₈/Al₈ and Na₈ with Fe₈, and wider ranges of Ca₈/Al₈, Na₈, Fe₈ and K/Ti than their host rocks, suggesting that these melt inclusions formed by mixing magmas of different melting degrees and depths. According to the average value and ranges of Ca₈/Al₈, Na₈, Fe₈ and K/Ti, these magmas would necessitate other mixing ends in shallow crust except in upper mantle. The compositional diversity of melt inclusions in MORBs phenocrysts cannot always be used to indicate magma mixing and crystallization in shallow crust, and melt inclusions in high Mg^# olivine formed under mantle pressure must be excluded in study of the magma process at crustal level. This study shows that, in EPR, MORBs have experienced mixing of magmas formed by different melting degrees and depths in the mantle.     

Bi掺杂O3型NaNi0.5Mn0.5O2钠离子电池层状正极材料的制备与储钠性能

O3型NaNi_0.5Mn_0.5O₂拥有高理论比容量且易于制备,是商业钠离子(Na⁺)电池的首选正极材料之一,但其循环稳定性仍面临挑战。利用Bi对NaNi_0.5Mn_0.5O₂进行改性。研究发现,Bi的引入可以在晶粒生长过程中通过调节表面能实现晶粒细化,并且Bi的掺杂增加了层状正极材料的晶胞参数,为Na⁺提供了宽的扩散通道,提高了Na⁺的扩散能力,优化了Na⁺在脱嵌过程中的可逆性。改性后的NaNi_0.495Mn_0.5Bi_0.005O₂实现了在2.0～4.0 V的电势区间内0.2 C倍率下的可逆容量为138.1 mAh/g,在5 C倍率下循环100圈后容量保持率可以达到97%。     

Effect of Na+ on xonotlite crystals in hydrothermal synthesis

The effect of Na⁺ ion concentration on the crystalline phase composition and morphology of xonotlite crystals prepared in a CaO-SiO₂-H₂O system via hydrothermal synthesis was analyzed. X-ray diffraction (XRD) and scanning electron microscopy (SEM) results indicate that Na⁺ ion concentration has a significant impact on the composition and morphology of crystalline phases in the products under the initial conditions of a molar ratio of CaO/SiO₂ of 1.0 and a reactant concentration of 0.05 mol·L^?1 at 225°C for 15 h. The main crystalline phase in the products has a phase transition from xonotlite to pectolite, and the morphology changes from fibrous to broomlike shape with the Na⁺ ion concentration increasing. Therefore, the content of Na₂O in the raw material should be less than 5wt% for preparing pure xonotlite crystals via hydrothermal synthesis in a CaO-SiO₂-H₂O system.     

Permian volcanisms in eastern and southeastern margins of the Jiamusi Massif, northeastern China: zircon U-Pb chronology, geochemistry and its tectonic implications

LA-ICP-MS zircon U-Pb dating and geochemical data for the Late Paleozoic volcanic rocks from eastern and southeastern margins of the Jiamusi Massif are presented to understand the regional tectonic evolution. Zircons from eight representative volcanic rocks are euhedral-subhedral in shape and display striped absorption and fine-scale oscillatory growth zoning as well as high Th/U ratios （0.33-2.37）, implying a magmatic origin. The dating results show that the Late Paleozoic volcanic rocks in the study area can be divided into two stages, i.e., the Early Permian （a weighted mean 205^Pb/238^U age of 288 Ma） and the Middle Permian volcanisms （a weighted mean 205^Pb/238^U age of 268 Ma）. The former is composed mainly of basalt, basaltic-andesite, andesite and minor dacite. They are characterized by low SiO2 contents, high Mg^# （0.40-0.59）, enrichment in Na （Na2O/K2O = 1.26-4.25） and light rare earth elements （LREEs）, relative depletion in heavy rare earth elements （HREEs） and high field strength elements （HFSEs）, indicating that an active continental margin setting could exist in the eastern margin of the Jiamusi Massif in the Early Permian. The latter consists mainly of rhyolite and minor dacite with high SiO2 （77.23%-77.52%）, low MgO （0.11%-0.14%）, enrichment in 1（20 （Na2O/K2O ratios 〈 0.80） and Rb, Th, U and depletion in Eu, Sr, P and Ti, implying a crust-derived origin. Therefore, it is proposed that the Middle Permian volcanic rocks could have formed under the collision of the Jiamusi and the Khanka Massifs.     

Recent high-resolution glaciochemical record from a Dasuopu firn core of middle Himalayas

A 16.8 m firn core of middle Himalayas was recovered on the col of Dasuopu glacier in August 2006, being 7000 m above sea level. A total of 317 samples were measured for stable oxygen isotope ratios （6180） and major ion concentrations （Na＋, NH＋, K＋, Mg2＋, Ca2＋, Cl-, SO4^2-, and NO3^-. The firn core dating and seasonal partitioning were carried out based on the marked seasonal variations along the stable oxygen isotopes and crustal species （Ca2＋, Mg2＋） profiles. The multi-parameters and high-resolution glaciochemical data set of Dasuopu firn core recorded the detailed chemical characteristics of pre cipitation in high-elevation region, middle Himalayas, since 1991 A.D., which mainly originated from the crustal and anthropogenic sources, while the sea-salt contribution was minor. The seasonal variability of major ion concentrations was dominated by the seasonal alternation of the prevalent air mass, atmospheric circulation situation and precipitation regime. Linear regression analysis indicated that most of the variance in annual ionic fluxes can be explained by a linear dependence on snow accumulation rate.     

The seasonal variations of δ~(18)O , Cl~- , Na~+ , NO_3~- and Ca~(2+) in the snow and firn recovered from Princess Elizabeth Land, Antarctica

Snow and firn samples recovered from two snow pits (2.5 and 4.5m deep) and one 50-m firn core along the route of the 1996/1997 Chinese First Antarctic Inland Traverse Expedition in Princess Elizabeth Land, East Antarctica, have been measured for chemical composition and oxygen isotope ratio. In the two snow pits, the variations of NO3- are partly in phase with that of δ18O, while the variations of Cl~ and Na+ are in inverse phase with that of δ18O. The variations of CI- , Na+ , NO3- and δ18O show obvious seasonal variations and annual stratag-raphy. However, with the depth increasing, the seasonal variations of δ18O are gradually smoothed below 3 m (corresponding to about 10-year mass accumulation) in depth while the seasonal variations of Cl- , Na+ and NO3- are kept fairly well in the whole profile of the 50-m firn core (corresponding to about 250-year mass accumulation). The results provide a useful tool for dating the snow stratum in this region. On the contrary, no obvious seasonal variations of Ca2 + are found in the profiles.     

Coupled isomorphic substitution and exsolution of pyroxene,rutile, apatite and quartz in supersilicic garnet

Dissolution of pyroxene in garnet at ultrahigh pressures produces supersilicie garnet with the coupled substitutions of Si^Ⅵ M^Ⅵ= A^Ⅵ A^Ⅵ and Si^Ⅵ Na^Ⅷ=A^Ⅵ M^Ⅷ,which are enhanced by rising pressure. The supersilicic garnet and exsolution of pyroxene, rutile, apatite and quartz in garnet during decompression were found in natural rocks,pointing to the importance in studying mantle-derived rocks and ultrahigh pressure metamorphism related to plate deep subduction. Ti, P, K and H2O enters garnet via the substitutions of Ti = Si, P^Ⅵ Na^Ⅷ = Si^Ⅵ CaⅧ, Si^Ⅵ K^Ⅷ = AI^Ⅵ M^Ⅷ, and [(OH)4]^4- = [SiO4]^4- or [4H]^4 = Si^4 respectively. The possible entering of Eskola pyroxene component M0.5AlSi2O6 in clinopyroxene, together with the common pyroxene component M2Si2O6, into garnet can lead to the presence of the substitution of Si^Ⅵ 0.5□^Ⅷ= A^Ⅵ 0.5M^Ⅷ in garnet structure, which plays a key role in the exsolution of rntile, apatite and quartz in garnet. Two new breakdown reactions are thus proposed on the basis of the new coupled substitution, which can be regarded as a theoretical model for the exsolntion of the 3 minerals in garnet. The real exsolution may be a combination of several breakdown reactions.     

TiO<Subscript>2</Subscript>@MgO core-shell film: Fabrication and application to dye-sensitized solar cells

In this study,TiO2@MgO core-shell film was obtained by using a simple chemical bath deposition method to coat a thin MgO film around TiO2 nanoparticles. The core-shell configuration was characterized by X-ray diffractometer (XRD),scanning elec-tron microscopy (SEM),energy dispersive X-ray spectroscopy (EDX),and high-resolution transmission electron microscopy (HRTEM). Lattice fringes were observed for the TiO2 particles,and the MgO shell showed an amorphous structure,revealing a clear distinction between the core and shell materials. Applying the core-shell film as photoanode to the dye-sensitized solar cells (DSSCs),it shows a superior performance compared to the pure TiO2 electrode. Under the illumination of simulated sunlight (75 mW-cm-2),the short circuit photocurrent (Jsc),the open circuit photovoltage (Voc),and the fill factor (fF) are 8.80 mA-cm-2,646 mV,and 0.69,respectively,and the conversion efficiency (η) in-creased by 21.8% (from 4.32% to 5.26%) when dipping for opti-mum condition.     

Surface chemical structure of titania-silica nanocomposite powder

Titania-silica （TS） nanocomposite powder with three different composite structures, containing 10-30 mol% SiO2 in each structure, have been prepared by sol-gel processes. The surface characteristics of these titania-silica samples have been investigated by X-ray photo-emission spectroscopy （XPS） and high resolution transmission electron microscopy （HRTEM）. The study for all TS oxides annealed at 773 and 1173 K showed： an abnormal surface enrichment in Si increased with increasing annealing temperature; the Ti^3＋, Ti^2＋, Si^3＋ and Si^2＋ oxides coexisted with Ti^4＋ and Si^4＋ oxides, and the contents of these Ti/Si suboxides increased with increasing SiO2 content and annealing temperature; there was a layer rich in O on the topmost surface and the excess O could be attributed to the chem-adsorption of H2O; different composite structures could lead to different contents of Ti/Si suboxides. These results indicated that the surface of TS oxide powder derived by sol-gel process was a double layer with enriched O first and then SiOx/TiOy（x, y〈2）. Ti/Si suboxides could result from the thermal diffusion of Ti^4＋ and Si^4＋, which might be induced by the strong interaction between Ti^4＋ and Si^4＋.     

Preparation,crystal structure and quantum chemical investigation of [Li(NTO) (H2O)]

[Li(NTO)(H₂O)₂] was prepared by mixing the aqueous solution of 3-nitro-1,2,4-triazol-5-one (NTO) and lithium hydroxide. The crystal structure of [Li(NTO)(H₂O)₂] was determined by single crystal diffraction analysis. The crystal is monoclinic, space group P2₁/n with crystal parameters of a = 0.742 0(2) nm, b = 0.344 9(1) nm,c = 2.490 6(3) nm, β= 94.89(1)°, Z = 4,D _c , = 1.799 g cm⁻³,V = 0.635 nm³, μ = 1.591 cm⁻¹, F(000) = 392. The finalR is 0.051. The MNDO MO calculation shows that the coordinate bonds of title compound possess certain extent of covalent character. O₂ atom of NTO anion is bonded to Li atom; the nitro group will be lost first when NTO is decomposed.     

Heteroseneous oxidation of carbonyl sulfide on mineral oxides

Heterogeneous oxidation of carbonyl sulfide （OCS） on mineral oxides including SiO2, Fe2O3, CaO, MgO, ZnO and TiO2, which are the main components of atmospheric particles, were investigated using in situ diffuse reflectance infrared Fourier transform spectroscopy （in situ DRIFTS）, ion chromatography （IC）, temperature-programmed desorption （TPD）, X-ray diffraction （XRD） and Brunauer-Emmett-Teller （BET） methods. The main products and intermediates of the heterogeneous oxidation of OCS on these oxides were identified with in situ DRIFTS and IC. The reaction mechanism and kinetics were also discussed. It is found that the reaction mechanism on these mineral oxides is the same as that on Al2O3 for the same final products and the intermediates at room temperature. Namely, OCS can be catalytically oxidized to produce surface SO4^2- species and gaseous CO2 through the surface hydrogen thiocarbonate （HSCO2-） and HSO; species. The activity series for heterogeneous oxidation of OCS follows： Al2O3 ≈ CaO 〉 MgO 〉 TiO2 ≈ ZnO 〉 Fe2O3 〉 SiO2. The specific area, basic hydroxyl and surface basicity of these oxides have effect on the reactivity. This study suggests that heterogeneous reactions of OCS on mineral dust may be an unneglectable sink of OCS.     

PbxNayYzF2x+y+3z+3m∶Erm3+上转换发光粉的低温燃烧合成及表征

采用低温燃烧合成（LCS）法一步合成了Pb_xNa_yY_zF_2x+y+3z+3m:Er_m3+氟化物体系1 550 nm响应的红外上转换发光材料. 通过正交实验研究了4种阳离子影响发光性能的主次关系及最佳配比,研究了燃料用量对晶相形成及上转换发光性能的影响. 采用X射线粉末衍射仪、透射电镜、荧光分光光度计（耦合1 550 nm激光器）等手段对样品的物相、形貌及发光性能进行了测试与表征. 结果表明:阳离子含量对红光发射强度影响的主次关系为Y3+,Pb2+,Na+,Er3+,最佳配比为Pb_0.004Na_0.003 Y_0.003 F_0.032:Er3+_0.004. 燃料取2.5倍理论用量时样品的结晶度和发光强度最高.      

1株嗜碱放线菌的生理学特性研究及其鉴定

 对从青海茶卡盐湖岸土样中分离到的1株生理较特殊的嗜碱放线菌YIM80305的生长pH范围,不同碱性物质KOH,K₂CO₃,NaOH,Na₂CO₃对其生长的影响,耐NaCl,KCl特性进行了研究.同时从形态,细胞壁类型,16SrDNA等方面进行了鉴定.结果发现YIM80305对Na⁺碱性物质有一定依赖性,对K⁺敏感,YIM80305可能是Streptomyces属的1个新种.     

Phase analysis and thermal conductivity of in situ O′-sialon/β-Si3N4 composites

Typical O??-sialon-based ceramics, with a formula of Si_2?x Al _x O_1+x N_2?x , where x was set as 0.25, were fabricated by in-situ synthesis. Si₃N₄, Al₂O₃, and SiO₂ powders were used as raw materials, and MgO and Y₂O₃ were added as sintering additives. All the samples were sintered at different temperatures under a nitrogen pressure of 0.25?C0.30 MPa, and their microstructure, phase content, and thermal conductivity were evaluated. The effects of O??-sialon and ??-Si₃N₄ on the thermal conductivity were analyzed by numerical calculation in detail. In the case of the similar porosity, the thermal conductivity of O??-sialon-based ceramics decreased with the ratio of O??-sialon/??-Si₃N₄ increasing. When the ratio was 12, the thermal conductivity of O??-sialon ceramics sintered at 1360°C was 1.197 W·m^?1·K^?1.     

Microstructure, crystalline phase and electrical properties of Li0.06(Na0.5K0.5)0.94Nb(1−2x/5)Mg x O3 lead-free piezoelectric ceramics

MgO-modified Li_0.06(Na_0.5K_0.5)_0.94NbO₃ (L₆NKN) lead-free piezoelectric ceramics were synthesized by normal sintering at a relatively low temperature of 1000°C. The crystalline phase, microstructure, and electrical properties of the ceramics were investigated with a special emphasis on the influence of MgO content. The addition of MgO effectively improves the sinterability of the L₆NKN ceramics. X-ray diffraction analysis indicates that the morphotropic phase boundary (MPB) separating orthorhombic and tetragonal phases for the ceramics lies in the range of Mg doping content (x) from 0.3at% to 0.7at%. High electrical properties of the piezoelectric constant (d ₃₃=238 pC/N), planar electromechanical coupling coefficient (k _p=41.5%), relative dielectric constant (? _r=905), and remanent polarization (P _r=38.3 μC/cm²) are obtained from the specimen with x=0.5at%, which suggests that the Li_0.06(Na_0.5K_0.5)_0.94Nb_(1?2x/5)Mg _x O₃ (x=0.5at%) ceramic is a promising lead-free piezoelectric material.