Sol-gel derived silicate oxyapatite phosphor films doped with rare earth ions

Rare-earth (Eu3+, Tb3+)-doped Ca2Y8(SiO4)(6)O-2 luminescent thin films were dip-coated on silicon and quartz glass substrates through a sol-gel route. X-ray diffraction (XRD), scanning electron microscopy (SEM) and luminescence excitation and emission spectra as well as luminescence decays were used to characterize the resultant films. The results of XRD reveal that these films remain amorphous below 700 degreesC, begin to crystallize at 800 degreesC, and crystallize completely around 1000 degreesC with an oxyapatite structure. The grain structure of the film can be seen clearly from SEM micrographs, where particles with various shape and average size of 250 nm can be resolved. The Eu3+ and Tb3+ ions show their characteristic red (D-5(0)-F-7(2)) and green (D-5(4)-F-7(5)) emission in the films with a quenching concentration of 10 and 6 mol% (of Y3+), respectively. The lifetime of Eu-3divided by increases with the heat treatment temperature front 700 to 1100 degreesC.

Sol-gel deposition of calcium silicate red-emitting luminescent films doped with Eu3+

Eu3+-activated calcium silicate (CaO-SiO2:Eu3+) luminescent films were prepared by the sol-gel method. The structural evolution of the film was studied by X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM), and the luminescence properties of the phosphor films were investigated as a function of heat treatment temperature. The XRD study indicates that a kilchoanite phase forms in the film sintered at 800 degreesC, which is different from that in gel powder treated under the same conditions. The SEM results show that the film thickness decreases and the particles in the film become smaller with increasing heat treatment temperature. The CaO-SiO2:Eu film shows the characteristic emission of Eu3+ under UV excitation, with the Eu3+ D-5(0)-->F-7(2) band (616 nm) being the most prominent. A large difference in the Eu3+ lifetime is observed between the film samples treated at 500 and 700 degreesC (or above). Concentration quenching occurs when the Eu3+ doping concentration is above 6 mol% of Ca2+ in the film.

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.

Luminescence of Pb2+ and energy transfer from Pb2+ to rare earth ions in silicate oxyapatites

The Pb2+ luminescence in a series of silicate oxyapatites Me(2)(Y, Gd)(8)(SiO4)(6)O-2, Me(4)Y(6)(SiO4)(6)O (Me = Mg: Ca, Sr) is reported and discussed in relation to the crystal structure. The maximum wavelengths of the excitation (S-1(0)-P-3(1)) and emission (P-3(1)-S-1(0)) bands of Pb2+ are independent of the Mc:Y ratio (2:8 or 4:6) but they have lower energies in MgY-oxyapatites than in CaY- and SrY-oxyapatites. The Stokes shift of Pb2+ luminescence amounts to 11 100 to 11 400 cm(-1): which does not depend strongly on the host composition. There exists a mutual energy transfer between Pb2+ and Gd3+ in Sr2Gd8(SiO4)(6)O-2. At last, the dependence of the energy transfer efficiency of Pb2+-Sm3+, Tb3+: Dy3+ in Sr-2(La: Gd)(8)(SiO4)(6)O-2 and Ca-2(Y, Gd)(8)(SiO4)(6)O-2 on their doping concentrations was studied in more detail.

Characteristics of anodic coatings oxidized to different voltage on AZ91D Mg alloy by micro-arc oxidization technique

With increasing applied voltage, three types of anodic coatings, passive film, micro-spark ceramic coating and spark ceramic coating were made by micro-arc oxidization (MAO) technique on AZ91D magnesium alloy in alkali-silicate solution. The structure, composition characteristics and the electrochemical properties of coatings were also studied with SEM, XRD and EIS (electrochemical impedance spectroscopy) technique, respectively. It is found that the electrochemical properties are closely related to the structure and composition characteristics of the anodic coatings. At the same time, the characteristics of the three types of anodic coatings differ significantly, among them, the micro-spark ceramic coating, prepared in the voltage range of 170similar to220V exhibits compact, homogeneous structure and highest corrosion-resistance.

东天山镁铁-超镁铁岩铜镍硫化物矿床通道式成矿机制与岩体含矿性评价研究

A mafic-ultramafic complex belt well developed in Eastern Tianshan, Xinjiang, NW China, which contains a series of Cu-Ni sulfide deposits. This area is the important production basis for Cu-Ni deposits, including Tulargen deposit, Hulu deposit, Huangshan-Huangshandong deposit, Hulu deposit, Xiangshan deposit, Tianyu deposit, Chuanzhu deposit. In China, especially Eastern Tianshan, it is prevalent that large Cu-Ni deposits occurred in small intrusions, typically including Jinchuan, Kalatongke, et al., so the ore-forming mechanism and evaluation rule for those small intrusions are very meaningful and of universal significance. On the basis of the research to typical Cu-Ni deposits, ore-forming conditions and processes are summarized through which to evaluate the ore-bearing potential for barren intrusions and unexplored mafic-ultramafic intrusions. By the contrast, metallogenic rule and mechanism of ore genesis are concluded, and evaluation system is preliminarily set up on the basis of these conclusions. Quantitatively simulation for the composition of olivine is introduced for the first time in China to discuss the interaction between magma and sulfide, and a new method to calculate the Mg-Fe composition of primitive magma is developed. Interaction between magma and sulfide liquid is used to get the Ni content in sulfide liquid. Sulfur isotopic characteristics in sulfide minerals in country rocks and ores are used to judge crustal sulfur introduction, which is applied for the first time in China. Re-Os isotopic characteristics are related to the ore-forming process, to interpret the process of enrichment of chalcophile elements. On the basis of the evaluation system, Mati, Chuanzhu, Luodong, Xiadong, those intrusions are evaluated to their ore-bearing potential. According to the studies to typical Cu-Ni deposits, conduit-type ore-forming model is set up, and the characteristics of the model are concluded systematically. The evaluation system and conduit-type ore-forming model can be helpful to the evaluation of mafic-ultramafic intrusions in this and similar mafic-ultramafic intrusion belts. The studied typical deposits and mafic-ultramafic intrusion include Tulargen deposit, Hulu deposit, Huangshandong deposit, Chuanzhu deposit, Mati intrusion，Luodong intrusion, Xiadong intrusion, and others. Through studies, there are similar characteristics for Tulargen and Hulu deposits in magma origin, composition of primitive magma（MgO=12.5%, FeO=12% and MgO=11%, FeO=10.5% respectively）, magma evolution, mechanism of sulfide segregation and conduit-type ore-forming process. By Re-Os isotopic system, the ore forming date of Tulargen deposit is 265.6±9.2Ma, which is consistent to regional metallogenic event, but little younger. The Mg-Fe composition of primitive magma of Baishiquan, Huangshandong area, Kalatongke is lower than that of Tulargen and Hulu deposit, showing common basalt composition. The Mg# value（Mg#=(Mg/Mg+Fe）increases gradually from Kalatongke to Baishiquan to Huangshan-Huangshandong East. Baishiquan intrusions show relatively higher crustal contamination by evidence of trace element, which indicates the lower magma original source, from depleted mantle to crust. One break is the discovery of komatiitic intrusion, Xiadong intrusion, which shows characteristics of highly magnesium (Max Fo=96). The primitive magma is calculated of MgO=28%，FeO=9%, belonging to komatiitic magma. Tectonic evolution of Eastern Tianshan is discussed. By the statistics of ore-forming data of porphyry copper deposits, magmatic sulfide Cu-Ni deposits, orogenic hydrothermal gold deposits, we believe that those deposits are the successive products of oceanic subduction, are and back-arc basin collision and post-orogenic extention. And Cu-Ni sulfide deposits and orogenic gold deposits occurred in the stage of post-orogenic extention. According to the conclusions, the conduit-type ore-forming mechanism of magmatic sulfide deposit is set up, and its characteristics and conditions are concluded as well. The conduit-type ore-forming system includes magma generation, sulfide segregation, enrichment of chalcophile elements, interaction of sulfide and magma, sulfide collection in limited space in magma conduit and bottom of the chamber, which make a whole ore-forming system.The ore-forming process of Cu-Ni sulfide deposits is concluded as three steps: 1. mantle derived magma rises upward to the middle-upper crust; 2. magma suffers crustal contamination of different degrees and assimilates crustal sulfur, which leads to sulfur saturation and sulfide segregation. Sulfide liquid interacts with magma and concentrates chalcophile elements; 3. enriched sulfide located in the conduit(Tulargen) or bottom of the chamber (Hulu). Depleted magma rises upward continuously to form barren complexes. For the practical cases, Tulargen deposit represents the feeding conduit, and Hulu deposit represents the bottom of the staging magma chamber. So the deeper of west of Tulargen and southwest of Hulu are the favorite locate for ore location. The evaluation for ore potential can be summarized as follows: (1) Olivine can be served as indicator for magma evolution and events of sulfide segregation; (2) Sulfur isotopic characteristics is an efficient method to judge sulfur origin for magmatic sulfide deposit; (3) Re-Os content of the ores can indicate interaction between sulfide and silicate magma and crustal contamination; (4) PGE mineralization is effected by degree of partial melting of mantle; (5) Cu/Zr is efficient parameter to judge sulfide segregation; (6) The effects of multiple magma fractionation and emplacement are important, for inverse order shows the destruction to previous solid lithofacies and orebodies. Mati, Chuanzhu, Xiadong, Luodong, mafic-ultramafic intrusions are evaluated using evaluation system above. Remarkable Ni depletion is found in olivine of Mati, and southwest of the intrusion can be hopeful location for ore location. Chuanzhu intrusion has remarkable evidence of sulfide segregation, but the intrusion represents the narrow feeder conduit, so the wide part of the conduit maybe the favorite location for sulfide to deposit. The ore potential of Luodong and Xiadong is not good. Both the intrusions show no Ni depletion in olivine, and there is no sulfide in country rocks, so no crustal sulfur is added into the magmatic system. For Sidingheishan, a very large intrusion, the phenomenon of sulfide segregation is found, but there are no favorite places for sulfide to deposit. So the Cu-Ni ore potential maybe not good, but PGE mineralization should be evaluated further.

Nitridation of magnesium powder of nanometric size from the thermal decomposition of magnesium anthracene

Highly reactive magnesium powder of nanometric size, which was generated by the thermal decomposition of magnesium anthracene . 3THF under vacuum, can react with N-2 under atmospheric pressure, even at 300 degrees C, to form magnesium nitride. The rate and extent of the reaction can be improved effectively by doping the magnesium powder with a small amount of nickel or titanium compounds.

Synthesis of nanometric-size magnesium nitride by the nitriding of pre-activated magnesium powder

Magnesium nitride (Mg3N2) was synthesized by the reaction of magnesium in the highly reactive form (Mg*) with nitrogen at 450 degrees C under normal pressure. The effect of doping with nickel dichloride on the nitridation of Mg* was investigated. Differential thermal analysis (DTA) of Mg* systems and transmission electron microscopy (TEM) measurement of the product formed were carried out. TEM measurement showed that the particle size of the Mg3N2 synthesized was in the nanometric range. The dependence of nitridation of the NiCl2-doped Mg* on temperature was investigated at temperatures ranging from 300 to 500 degrees C. The nitridation of NiCl2-doped Mg* could occur even at temperature as low as 300 degrees C. (C) 1999 Kluwer Academic Publishers.