溶胶—凝胶法制备（Pb,Cd,La）TiO3薄膜及其特性

采用溶胶－凝胶法及均胶工艺,分别在石英玻璃和硅单晶上制备（Ｐｂ,Ｃｄ,Ｌａ）ＴｉＯ２薄膜。用ＳＥＭ分析薄膜的形貌,用ＦＴ－ＩＲ及ＤＴＡ等技术对ＰＣＬＴ薄膜及凝胶粉晶化情况进行分析。用ＸＲＤ对不同基片、不同厚度薄膜成相的影响进行了分析讨论。     

Evaluation of the distribution patterns of Pb, Cu and Cd from MSWI fly ash during thermal treatment by sequential extraction procedure

Municipal solid waste incinerator (MSWI) fly ash was frequently classified as hazardous materials as the metals' concentration of toxicity characteristic leaching procedure (TCLP) exceeded regulations. Many studies have focused on reducing the concentration of TCLP using thermal treatment and increasing the application of thermally treated slag. However, the metal patterns in MSWI fly ash with or without thermal treatment have seldom been addressed. The main objective of this study was evaluation of the distribution patterns of Pb, Cu and Cd from MSWI fly ash during thermal treatment by sequential extraction procedure. The experimental parameters included the form of pretreatment, the proportion of bottom ash (bottom ash/fly ash, B/F=0, 0.1 and 1) and the retention time. The results indicated that (1) In comparison to raw fly ash, the distribution patterns of Pb, Cu and Cd become stable in thermally treated slag. (2) Washing pretreatment caused the Pb pattern to become stable, while the influence on Cu and Cd were not significant. (3) The distribution patterns of Pb, Cu, and Cd became more stable as the retention time increased. (4) Adding bottom ash could make the distribution patterns of Pb and Cd more stable.     

PbBr2-PbF2-P2O5玻璃的结构研究

采用红外光谱（IR）和X射线光电子能谱（XPS）等方法研究了PbBr2-PbF2-P2O5系铅卤磷酸盐玻璃的结构。结果表明，Pb^2 离子在玻璃中起着网络修饰阳离子和网络形成体的双重作用。当P2O5含量为60mol%时，Pb^2 离子主要是作为网络修饰体；当P2O5含量降低到50mol%时，一部分Pb^2 离子能够进入玻璃网络形成[PbO4]四面体或P－O－Pb键。Br^-和F^-离子达到一定浓度时就会进入玻璃网络，形成[PO4-nXn](X=Br或F，n=0-4)四面体使磷酸盐链长变短。玻璃中P2O5的含量不变时P－O－P键的比例也基本保持不变；当P2O5的含量降低时，P－O－P键和P－O^-键的含量都减少，P－O－Pb键的含量则明显增加。     

CdF2-BaF2-LiF系统玻璃的X射线衍射与分子动力学研究

采用无水氟化物直接熔化法得到了CdF2－BaF2－LiF系统玻璃的玻璃形成区，用X射线衍射和分子动力学计算机结构模拟等手段研究了成分为36CdF2－34BaF2－30LiF（mol％）的玻璃的结构．研究表明，Cd原子主要为6、7和8配位，Ba原子主要为8配位，Cd－F的平均键长为2.29玻璃结构可以看作是由Li 连接的[CdF72]多面体共边或共角堆积而成．Cd－Cd键长在共边连接时为3.52共角时为4.03对氟化物玻璃中Li 原子所起的作用进行了比较．     

The effect of Fe contents on the local structure and crystallization behavior of SiO<Subscript>2</Subscript>–CaO–P<Subscript>2</Subscript>O<Subscript>5</Subscript>–Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses

The glass and glass ceramics containing SiO₂–CaO–Fe₂O₃–P₂O₅ were prepared by sol–gel method. The influence of the Fe contents on the crystallization and local structure of the glass and glass ceramics was systematically investigated. The crystal structure of the glass ceramics was identified by XRD characterization. Hematite phase can be precipitated from the glass matrix in all glass ceramics with various Fe contents, and the crystallographic parameters of hematite were determined by XRD Rietveld refinement. The crystallization kinetics of the glasses was investigated in detail. Relative low activation energies were obtained at low Fe contents. The local structure evolution of the glass and glass ceramics has been studied in-depth by means of FTIR and Mössbauer spectroscopy. Fe element is present both as network former and network modifier which significantly influenced the crystallization activation energies of the glasses. The results of this work may be of great significance for the material design and practical applications of bioactive magnetic glass ceramics for hyperthermia.     

Structural and optical properties of the SiO2-P2O5 films obtained by sol-gel method

A comparative study of the sol-gel films prepared in the SiO₂-P₂O₅ system starting with triethylphosphate, triethylphosphite and phosphoric acid as P precursors was performed. The work addresses basic aspects of physics, chemistry, and engineering of oxide films for applications in microelectronics, sensing, nano-photonics, and optoelectronics by establishing the influence of different precursors on the composition, structure and optical properties of the obtained films. The influence of the type of substrate (glass and indium tin oxide coated glass) and of the thermal treatment (200 and 500 °C) on their structure and properties was studied. By spectroscopic ellipsometry, X-Ray photoemission spectroscopy and atomic force microscopy measurements the high vaporization of the phosphorous during the densification of the films by thermal treatment was noticed when P-alkoxides were used. The phosphoric acid that forms chemical bond with silica network during the sol-gel process leads to better incorporation of P in the silica network as compared to the P-alkoxides.     

BaFe12O19/SiO2-B2O3-K2O 微晶玻璃陶瓷的低温合成及其微波性能

采用柠檬酸sol-gel工艺合成了BaFe₁₂O₁₉/SiO₂-B₂O₃-K₂O微晶玻璃陶瓷, 并对其介电常数及其磁导率在100MHz～ 6 GHz 下的变化规律进行了研究。结果表明: BaFe₁₂O₁₉/SiO₂-B₂O₃-K₂O微晶玻璃陶瓷可以在850℃/5 h的条件下烧结而成, 其合成过程与体系中的Ba/Fe 密切相关; 其介电常数基本不随测试频率的变化而变化; 其磁导率实部随测试频率的增加而下降。      

Raman Spectrum and Thermal Stability of a Newly Developed TeO2-BaO-BaF2-La2O3-LaF3 Glass

In this work, a new TeO2-BaO-BaF2-La2O3-LaF3 oxyfluorotellurite glass system is investigated. Differential thermal analysis (DTA) and structural analysis by Raman scattering spectra are reported on the glasses. The DTA results indicated that an increase of fluoride content in the glasses decreases the glass transition temperature (Tg) and increases the crystallization onset temperature (Tx). As a result the 70TeO2·20BaF2·10LaF3 glass showed a large Hruby's parameter, possessing excellent thermal stability. Changes in glass network structure with fluoride content are discussed based on the Raman scattering spectra of glasses. The glass network structures in the 70TeO2·(20-x)BaO·xBaF2·(10-y)La2O3·y1 aF3 glasses are basically composed of both Te(O, F)4 and Te(O, F)3 units, but the Te(O, F)4/Te(O, F)3 ratio in the glass becomes higher with increasing fluoride content. This may be considered one of the reasons why the 70TeO2·20BaF2·10LaF3 glass exhibits excellent thermal stability.     

Na20-- A1203 -- SiO2微晶玻璃体系熔体结构的分子动力学模拟

采用分子动力学方法模拟了7种组分的Na20-- A1203 -- SiO2体系微晶玻璃熔体结构,分析了体系的径向分布函数、键长分布和键角分布,得出了不同含量Na＋对Na20-- A1203 -- SiO2体系玻璃网络结构的影响。     

Synthesis and characterization of low cost willemite based glass–ceramic for opto-electronic applications

This paper presents a comprehensive study on thermal, structural and optical properties of novel willemite glass–ceramics. The precursor glass in the ZnO–SLS glass system was successfully prepared using conventional melt-quenching technique and willemite (Zn₂SiO₄) glass–ceramics were derived from this precursor glass by a control crystallization process. The effect of heat-treatment temperature on the phase transformation, morphology and size of Zn₂SiO₄ crystal phase was examined using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) techniques. Furthermore, fourier transform infrared reflection (FTIR) spectroscopy was used to evaluate the Zn₂SiO₄ crystal structural evolution. The average size of Zn₂SiO₄ crystallite obtained from calculation of XRD is found to be in the range 30–60 nm, whereas the grain size observed in FESEM is in range of 200–400 nm. The appearance of SiO₂, ZnO₄ and Zn–O–Si bands detected from FTIR indicate the formation of Zn₂SiO₄ crystal phase. Besides, the study of the optical band gap has found that optical band gap of the glass–ceramics decreased as the heat treatment temperature increased. The photoluminescence spectra of willemite glass–ceramics exhibit two different emissions around 525 nm (green) and 585 nm (yellow); exhibit a characteristic of broad absorption band around 260 nm. These two different spectra reveal that the luminescence performance of the willemite glass–ceramics was enhanced with the progression of heat treatment temperature due to different located energy levels of the β-Zn₂SiO₄ and α-Zn₂SiO₄ crystalline phase. Such luminescent glass–ceramics was expected to find potential applications in phosphors and opto-electronic devices.     

晶化温度对齿科用微晶玻璃物理性能的影响

根据齿科CAD／CAM加工用修复材料的要求,采用K2O－MgO-MgF2-SiO2微晶玻璃系统,通过差热分析（DTA）、X射线衍射分析（XRD）、扫描电子显微镜（SEM）观测及物理性能测试,研究了3种不同晶化温度对四硅氟云母微晶玻璃的晶化特性、微观结构及物理性能的影响。研究结果表明,随着晶化温度的逐步升高,四硅氟云母晶粒和径厚比逐步增大,抗弯强度和断裂韧性亦逐渐增高,维氏硬度和脆性指数随温度升高而降低;而提高晶化温度对密度无明显影响。     

B2O3-Li2O玻璃的制备与性能的研究

采用高温熔融法制备了不同配比的硼锂二元体系玻璃,并利用UVPC、NMR和DSC等手段研究了不同锂含量对玻璃透过率、结构和热稳定性的影响。结果表明:在硼酸盐玻璃中引入少量Li₂O,[BO₃]三面体会向[BO₄]四面体转变,使玻璃的网络结构有所加强,热稳定性提高,且玻璃中非桥氧数量降低,紫外透过率升高;当加入过量Li₂O时,产生断网结构,玻璃稳定性逐渐下降,非桥氧数量增加,导致紫外透过性能降低。     

溶胶-凝胶法制备SiO_2-TiO_2纳米复合薄膜紫外光处理的研究

采用溶胶－凝胶技术,结合二步水解法分别在单晶硅片、石英玻璃和Ｋｇ玻璃上制备ＳiＯ2、ＴiＯ2纳米复合薄膜,采用高压汞灯对其进行紫外光处理,分别用ＡＦＭ、椭偏仪、ＦＴＩＲ、ＵＶ－Ｖis分光光度计以及ＸＲＤ对凝胶膜紫外光处理前后的光学性能和结构进行研究,并与传统的热处理进行比较与分析．研究表明,紫外光处理是实现凝胶膜低温致密化的有效方法之一,其致密化的机理不同于传统的热处理,主要是通过紫外高能光子诱导复合薄膜网络结构的原子中的电子激发,导致原子化学键的断裂,进而产生结构重组而致密化．     

溶胶-凝胶法制备SiO2-TiO2纳米复合薄膜紫外光处理的研究

采用溶胶－凝胶技术,结合二步水解法分别在单晶硅片、石英玻璃和K9玻璃上制备SiO2-TiO2纳米复合薄膜,采用高压汞灯对其进行紫外光处理,分别用AFM、椭偏仪、FTIR、UV－Vis分光光度计以及XRD对凝胶膜紫外光处理前后的光学性能和结构进行研究,并与传统的热处理进行比较与分析。研究表明,紫外光处理是实现凝胶膜低温致密化的有效方法之一,其致密化的机理不同于传统的热处理,主要是通过紫外高能光子诱导复合薄膜网络结构的原子中的电子激发,导致原子化学键的断裂,进而产生结构重组而致密化。     

Effect of oxide dopant on the structure of fluorozirconate glasses studied by X-ray photoelectron spectroscopy

The effect of oxide dopant on the structure of 62ZrF₄-30BaF₂-8LaF₃ (mol%) glass by equimolar substitution of BaO for BaF₂ was studied by X-ray photoelectron spectroscopy (XPS). The XPS spectra of La 3d, Ba 3d, F 1s, O 1s and Zr 3d were measured. From the deconvoluted results for the XPS spectra of elements in the glass, it was proposed that the oxide ions added to the glass mainly bond to Zr⁴⁺ and replace the bridging fluoride ions resulting in the formation of the F-Zr-O bond. Further analyses indicated that the oxide ions mainly play a non-bridging role instead of a bridging role in the glass structure.     

Evaluation of binding selectivities of caged crown ligands toward heavy metals by electrospray ionization/quadrupole ion trap mass spectrometry

Electrospray ionization (ESI)/quadrupole ion trap mass spectrometry is used to evaluate the heavy metal binding selectivities of five caged crown ethers and two polyether reference compounds in methanol solution. The binding preferences for Hg2+, Pb2+, Cd2+, and Cu2+ were analyzed by comparison of ESI mass spectral intensities with the aim of developing this method for the rapid screening of binding selectivities of new synthetic ligands. The cage compounds preferentially bind Hg2+, except for the cage cryptand derivative, which favors Pb2+. The preference for Hg2+ stems from the favorable positioning of the nitrogen or sulfur atoms for linear coordination of Hg2+, whereas the cryptand derivative favors Pb2+ because of its larger cavity size. The counterions of the metal salts influence the type of complexes observed in the ESI mass spectra because the strengths of the metal-anion bonds affect retention of the anion in the complexes.     

Effects of fluorine on crystallization,structure and performances of lithium aluminosilcate glass ceramic

The effects of fluorine on the nucleation, crystallization, structure and performances of low-expansion lithium aluminosilcate glass ceramic are investigated by the differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and other measuring technologies. The introduction of fluorine promotes the nucleation and crystallization of LAS glass, lowers the crystallizing temperature, allows a direct formation of β-spodumene without the transformation from β-quartz into β-spodumene and as a result, refines the microstructure and improves the physical and mechanical properties of the glass ceramics.     

Structural properties of fluorozirconate-based glass ceramics doped with multivalent europium

The structure/property relationships of fluorochlorozirconate glass ceramics as a function of divalent and trivalent europium (Eu) co-doping and thermal processing have been investigated; the influence of doping ratio on the formation of barium chloride (BaCl(2)) nanocrystals therein was elucidated. X-ray absorption near-edge structure spectroscopy shows that the post-thermal annealing changes the Eu valence of the as-poured glass slightly, but during the melting process Eu(3+) is more strongly reduced to Eu(2+), in particular, when doped as a chloride instead of fluoride compound. The Eu(2+)-to-Eu(3+) doping ratio also plays a significant role in chemical equilibrium in the melt. X-ray diffraction measurements indicate that a higher Eu(2+) fraction leads to a BaCl(2) phase transition from hexagonal to orthorhombic structure at a lower temperature.     

氧化铋对微晶玻璃的相转变和性能的影响

为研究Bi2O3在堇青石基微晶玻璃烧结中的作用及其添加量对微晶玻璃的相转变和性能的影响,采用烧结法制备了不同Bi2O3含量的微晶玻璃,并对其进行了X射线衍射分析、显微分析和性能测试.结果表明:Bi2O3的加入降低了堇青石的u相向a相转变的温度,并有效促进微晶玻璃的烧结致密化;烧结样品的介电常数和抗折强度均随着Bi2O3加入量的增加而增加,且与密度变化规律相似;当Bi2O3添加量(质量分数)达5%时样品的介质损耗因子最低(＜10-3);微晶玻璃烧结样品的热膨胀系数基本符合线性规律.     

云母微晶玻璃等温转变动力学的研究

本文对以TiO₂为晶核剂的云母微晶玻璃等温析品转变进行了研究,发现玻璃的差热分析（DTA）曲线上出现了两个析晶放热峰,X光衍射分析（XRD）表明,在这两个析晶峰温度下从玻璃中分别析出了钛酸镁（MgTi₂O₅）和云母（KMg₃AlSi₃O₁₀F₂）晶体.用差热分析测定了玻璃等温析晶活化能和晶体的生长指数．玻璃析出钛酸镁和云母的活化能分别为242kJ／mol和265kJ／mol．云母晶体以二维方式生长,生长过程受界面过程控制.