乙二醇辅助聚乙烯醇制备花状氧化铈探索

利用浓硝酸和双氧水将不规则形貌氧化铈溶解，生成硝酸铈.采用水作为溶剂或水和乙二醇共同作为溶剂，聚乙烯醇作为分散剂，草酸铵作为沉淀剂，通过直接沉淀法合成草酸铈前驱体，在高温反应炉中按照8 ℃/min的升温程序，600 ℃保温2 h，得到氧化铈.结果表明，以水为溶剂，聚乙烯醇为分散剂时，所得氧化铈易碎，呈尺寸不均匀片状，厚度在100 nm左右，长度和宽度尺寸约3~10 μm和1~2 μm，比表面积为14.9 m2/g.以水和乙二醇共同为溶剂，聚乙烯醇为分散剂时，所得氧化铈具有花状结构，由表面光滑、尺寸均匀的纳米片组成，片状氧化铈的厚度、长度和宽度分别约100 nm、4 μm和1.5 μm，形成直径约2~5 μm的氧化铈花状团簇，比表面积为21.45 m2/g.利用乙二醇辅助聚乙烯醇制备花状氧化铈，有望应用于调节具有花状形貌的稀土氧化物.      

碳酸氢铵沉淀法制备氧化铈抛光粉

利用碳酸氢铵做沉淀剂制备氧化铈抛光粉,通过L16(44)正交试验,研究了温度、硝酸铈浓度、滴加速度和搅拌速度对氧化铈粒度和比表面积的影响。得到的最佳粒度制备工艺条件为:温度60℃、硝酸铈浓度50g/L、搅拌速率500r/min、滴加速度50mL/min。并对最佳制备工艺条件下制取的抛光粉进行粒度、形貌和抛蚀量进行研究。     

高松装比氧化铈的制备

对制备氧化铈沉淀剂的选择,沉淀因素影响及煅烧条件等工艺进行优化选择。试验证明：该工艺能生产出高松装比产品。     

碳酸盐沉淀法制备超细氧化铈的研究

研究了碳酸盐沉淀法制备超细氧化铈粉体的工艺。结果表明,采用碳酸盐正向沉淀法可以得到超细氧化铈粉体,其体积中心粒径D50为0.086μm、比表面积为59.489 m2.g-1,晶体结构为立方晶系,萤石型结构,形状为棒状,分散性较好。     

化学法提取氧化铈工艺研究

本文论述了用化学法提取氧化铈工艺进行的研究,提出了简便的从氟碳铈镧矿硫酸浸出液中分离纯铈的工艺流程,纯度可达99％以上。     

制备条件对大颗粒氧化铈流动性的影响

对草酸沉淀法和碳酸氢铵沉淀法制备大颗粒氧化铈的流动性进行了研究。在草酸沉淀法中,研究了搅拌速度、沉淀温度、陈化时间、沉淀剂的加入速度和灼烧温度等条件对C eO2流动性能的影响,这些制备条件对C eO2粉体的流动性影响不是很大,制得的大颗粒氧化铈的流动性指数介于70~80之间,流动性良好;碳酸盐沉淀法制备大颗粒C eO2,晶种和添加剂可以改善C eO2粉体的流动性,加入适量的晶种和添加剂,也可以制得流动性指数都介于70~80之间,流动性良好的大颗粒C eO2。     

氧化铈粒度控制研究

以碳化铈为前驱体,通过对沉淀条件的控制及填加剂的使用,控制碳酸盐的粒度,在850℃条件下灼烧后一次性得到D 50=4～7μm理想粒度的氧化铈,并可实现连续的工业化生产.     

以碳酸铈为前驱体制备超细氧化铈及其抛光性能

研究了以水合碳酸铈为前驱体,采用直接球磨和煅烧的方法制备了中位粒径小于3μm的超细氧化铈。结果表明:所得产物均具有立方萤石型结构,随着煅烧温度的升高,产物粒径呈下降趋势,粒度分布也越来越窄,结晶度提高。但对三种不同玻璃的抛光能力均在900℃~1000℃之间呈现出极大值。因此认为抛光过程中玻璃表面物质的去除速率受抛光粉粒度、结晶度和表面活性的影响较大。     

纳米粉制备过程中团聚现象的探讨

探讨了纳米粉体材料在制备过程中形成的团聚体的性质、产生团聚体的原因以及阻止团聚体形成的措施。     

pH对碳酸铈粒子团聚的影响

在不同的(NH4)2CO3和Ce(NO3)3摩尔比值R、初始料液Ce(NO3)3溶液的pH以及(NH4)2CO3加料时间条件下制备了Ce2(CO3)3粒子,并用SEM和Zeta电位仪对其进行表征。结果表明,溶液pH对Ce2(CO3)3粒子形貌无影响,只是使得溶液离子浓度及双电层厚度发生改变,进而引发Ce2(CO3)3粒子的团聚。当R=1.6、pH=4、加料时间1h时得到的Ce2(CO3)3形貌最好,颗粒分散性好。     

新型电荷转移配合物(C9H8N)10(NH4)3[Y(SiMo11O39)2]·20H2O的合成与表征

由三元杂多化合物(NH4)13[Y(SiMo11O39)2]·36H2O与喹啉反应合成了电荷转移化合物(C9H8N)10(NH4)3[Y(SiMo11O39)2]*20H2O.采用元素分析、X射线粉末衍射、红外光谱、固体漫反射电子光谱进行了表征.结果表明喹啉通过N原子结合质子形成阳离子与稀土杂多阴离子成盐,固体化合物中阴离子和阳离子之间存在较强的相互作用;化合物在光激发下发生分子内电荷转移,导致有机C9H8N+大阳离子的氧化和稀土杂多阴离子的还原,标题化合物颜色由黄转变为深蓝色.     

钴盐沉淀—热分解法制备超细八面体四氧化三钴

提出了一种以硫酸钴、碳酸氢铵为原料,聚乙二醇为表面分散剂,采用钴盐沉淀—热分解法制备超细八面体Co3O4的方法。通过热重-差热分析仪、红外光谱分析仪、X射线衍射仪、场发射扫描电镜、激光粒度分析仪对前驱体碱式碳酸钴和产品Co3O4进行了分析和表征。结果表明:制备的Co3O4粉末呈八面体晶体形貌,粒度在亚微米至微米级,粒度分布均匀且范围窄,制备过程分散剂的添加消除了粉末的团聚现象。     

Hydrothermal synthesis and crystal structure study of two novel 3-D mellitates {Nd2[C6（COO）6] （H2O）6} and {Ho2[C6（COO）6]（H2O）6}

Two novel 3-D coordination compounds, Nd2[C6（COO）6]（H2O）6 （1）and Ho2[C6（COO）6]（H2O）6 （2）, were hydrothermaily synthesized from mellitic acid and neodymium perchlorate （or holmium perchlorate） in the alkaline aqueous solution and characterized with elemental analysis, TG, IR spectrum, and single crystal X-ray diffraction. The two compounds were isostructural and crystallized in the orthorhombic system, space group Pnnm, with a=1.3531 （4） nm, b=0.6687 （2） nm, c=1.0224（3） nm, V=0.92523（5） nm^3, Z=4, D=2.630 g/cm^3, F（000）=696.0, Goof=1.052. Final R indices [1 〉2∑（Ⅰ）]： R1=0.0195, wR2=0.0382 for 1; a=1.3411 （2） nm, b=0.6586（1） nm, c=1.0116（2） nm, V=0.8935（3） nm^3, Z=4, D=2.877 g/cm^3, F（000）=724.0, Goof=1.061. Final R indices [1 〉2∑（Ⅰ）]： R1=0.0200, wR2=0.0479 for 2. In the two compounds 1 and 2, the mellitic acid ligand, in which all the carboxylate groups were deprotonated, had only one kind of coordination mode to bridge metal ions to form four-connected three-dimensional diamondiod networks.     

混合铜矿的常压氨浸与高压氨浸

对新疆某地的混合铜矿进行了常压氨浸和高氧压氨浸工艺研究,详细考察了NH3*H2O浓度、铵盐用量、氧化剂用量、氧压、浸出温度、浸出时间等因素对浸出过程的影响。结果表明,在常压、有氧化剂存在条件下,铜浸出率仅达到74.56%,而在高氧压条件下,铜的浸出率可达到98%。     

Effects of Cerium Oxide on Ni／Al2O3 Catalysts for Decomposition of CH4 and C2H4

Characteristics of carbon deposition of CH4 and C2H4 decomposition over supported Ni and Ni-Ce catalysts were studied by using a pulse reaction as well as BET, TPR, XPS and hydrogen chemisorption techniques. It is found that there is a metal-semiconductor interaction (MScI) in the Ni-Ce catalyst, and the effect of MScI on the carbon deposition of CH4 decomposition is opposite to that of C2H4. A novel model of carbon deposition of CH4 or C2H4 decomposition was proposed.     

Investigation on pumping oxygen characteristics of （Bi2O3）0.73（Y2O3）0.27 solid electrolyte

（Bi2O3）0.73（Y2O3）0.27 fine powders prepared by wet chemical precipitation method were cold isostatically pressed to form solid electrolyte tubes, and sintered at 900 ℃ for 10 h in the air. Their pumping oxygen characteristics in non-dehydrated Ar gas were investigated, where a ZrO2 （Y2O3 stabilized） oxygen sensor was used to measure the oxygen partial pressure Po2. The results showed that the Po2 value reached magnitudes of 1×10^-2-1×10^-10 Pa at the applied pumping oxygen voltage of 0.5 V, 1×10^-37-1×10^-27 Pa at 1.0 V and 1×10^-53-1×10^47 Pa at 2.0 V within the temperature range from 550 to 650 ℃. Moreover, no cracks were found in the tested solid electrolyte tubes. Thus, the Bi2O3-Y2O3 system might be used in solid electrolyte oxygen pump for purifying gases.     

Syntheses,characterization, and luminescence of two lanthanide complexes [Ln2（acetate）6（HeO）4]·4H2O （Ln=Tb（1）, Sm（2））

Two dinuclear compounds [Ln2（acetate）6（H2O）4]-4H2O （Ln=Tb（1）, Sm（2）） were obtained by the hydrothermal reaction of Ln2O3 with malonic acid at 150 ℃. Both compounds were characterized by elemental analyses, infrared spectra, and single crystal X-ray diffraction. The results showed that complexes 1 and 2 were isomorphous and crystallize in triclinic space group P 1. The coordination geometry around Ln（Ⅲ） ions in the complexes 1 and 2 was a distorted tricapped trigonal prism with a nine coordination. In the crystal, the molecular organization was further stabilized by well-defined weak hydrogen bonding interactions between the neutral dinuclear molecular units that led to the formation of a three-dimensional network. The fluorescence properties of the two complexes 1 and 2 in organic solvents were also studied. The results show that the ligand acetate favored energy transfer to the emitting energy level of Tb（Ⅲ） in complex 1. Some factors that influence the fluorescent intensity were also discussed in the article.     

Thermochemical Study on Ternary Solid Complex of La(Gly)2 (Ala)3 Cl3 ·2H2O (s)

The complex of lanthanum chloride with Glycine and Alanine, La(Gly)₂(Ala)₃Cl₃ · 2H₂O, was synthesized and characterized by IR, elementary analysis, thermogravimetric analysis, and chemical analysis. The dissolution enthalpies of LaCl₃ · 7H₂O(s), 2Gly(s) + 3Ala(s) and La(Gly)₂(Ala)₃Cl₃ · 2H₂O(s) were determined in 2 mol · L⁻¹ HCl by a solution-reaction isoperibol calorimeter. By designing a thermochemical cycle in terms of Hess' Law and through calculation, the reaction enthalpy of lanthanum chloride seven-hydrate with Glycine and Alanine was obtained: Δ_rH^θ_m(298.15 K) = (29.652 ± 0.504) kJ · mol⁻¹, and the standard enthalpy of formation of La(Gly)₂(Ala)₃Cl₃ · 2H₂O(s) Δ_fH^θ_m[La(Gly)₂ (Ala)₃Cl₃ · 2H₂O, s, 298.15 K] = −4467.6 ± 8.3 kJ · mol⁻¹.     

Morphology of dispersed nickel electrochemically deposited in solutions of the system NiSO4(NiCl2)-(NH4)2SO4-NH3·H2O

Morphology of dispersed nickel obtained by electrolysis in electrolytes (0.1–0.5 M) NiSO₄(NiCl₂)-0.5 M (NH₄)₂SO₄-NH₃·H₂O (to pH 8.0–8.5), which model the leaching solutions of secondary metal, is investigated. It is noted that the sediment of three structural levels is formed on the cathode at the current density 20–100 A/dm². These are (i) spherical particles, (ii) spherical agglomerates, and (iii) conglomerates of the particles of the second structural level. The shape of first-level elemental particles is governed by adsorption of the surface-active NH₃ molecules on the surface of crystalline nuclei. The second and the third levels of structuring emerge due to high surface energies of elemental particles. Spherical agglomerates are mechanically stable and determine the main characteristics of the nickel powder. The sizes of these agglomerates decrease as the cathode current density increases and the nickel concentration in electrolytes decreases, and lie in the limits 2–10 μm. Original Russian Text ? O.I. Kuntyi, 2007, published in Izvestiya VUZ. Tsvetnaya Metallurgiya, 2007, No. 1, pp. 20–23.     

Photoluminescent properties of Ca2Gd8（SiO4）6O2： Dy^3＋ phosphor films prepared by sol-gel process

There are growing interests on phosphor thin films owing to their potential application in high-resolution devices such as cathode ray tubes and flat panel display devices. The solution-based sol-gel method is one of the most important techniques for the synthesis of various functional coating films. Compounds with the apatite structure are very suitable host lattices for various luminescent ions. Ca2RE8（SiO4）6O2 （ RE=Y, Gd, La ） is a kind of ternary rare-earth-metal silicate with oxyapatite structure, which has been used as host material for the luminescence of various rare earth and mercury-like ions. In this article, Ca2Gd8（SiO4）6O2：Dy^3＋phosphor films were dip-coated on quartz glass substrates through the sol-gel process. X-ray diffraction （XRD）, atomic force microscopy （AFM）, photoluminescence （PL） spectra, as well as lifetimes were used to characterize the resulting films. AFM study revealed that the phosphor films consisted of homogeneous particles. The Dy^3＋ showed its characteristic emission in crystalline phosphor films, i.e., ^4F9/2-^6H15/2 and ^4F9/2-^6H13/2.