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A porous coordination polymer, {[Ce(dpdo)4(H2O)3](PMo_12O_40)(dpdo)0.5(H2O)4}n 1 (dpdo = 4,4'-bipyridine-N,N'-dioxide), templated by double-Keggin-type polyanions was synthesized and structurally characterized. The crystal structure was determined by single-crystal X- ray diffraction. The crystal is of triclinic, space group P1 with a = 13.368(4), b = 16.503(4), c = 18.506(5)А, α = 88.831(5), β= 82.095(5), γ = 83.578(5)°,V= 4018.6(18)А^3, Z=2, C45H50N9O56CeMo12P, Mr = 2935.31, Dc = 2.426 g/m^3, μ= 2.491 mm^-1, F(000) = 2816, the final R=0.0603 and wR = 0.1611 for 11977 observed reflections with I 〉 2σ(I). Compound 1 exhibits a 3D non-interwoven framework with large cavities housing centrosymmetrically related shoulder-by-shoulder double-Keggin anions as guests. 相似文献
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A new one-dimensional dicyanamide bridged zinc(II) complex containing nitronyl nitroxide radicals Zn(NO3)(NIT-1'-MeBzIm)(dca)n·(H2O)n(NIT-1'-MeBzIm = 2-{2'-(l'-me-thyl)benzimidazolyl}-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide, dca = dicyanamide anion) has been prepared and structurally characterized by single-crystal X-ray diffraction.The complex crystallizes in triclinic, space group P1, with a = 7.428(3), b = 9.839(3), c = 16.708(6), α = 93.270(4), β = 101.642(4), γ = 100.632(4)°, C17.5H21N8O5.5Zn, Mr = 496.79, V = 1169.7(7) 3, Dc = 1.411 g/cm3, μ(MoKα) = 1.096 mm-1, Z = 2, F(000) = 512, R = 0.0583 and wR = 0.1663 for 4295 observed reflections with I > 2σ(I).X-ray analysis reveals that the zinc(II) ion is six-coordinated with a distorted octahedral geometry.These units develop as 1D species where dicyanamide ligands bridge zinc(II) ions.In addition, molecules are linked by π-π piling interactions to form 1-D double-chains.Magnetic investigation indicates that the weak intramolecular interactions are antiferromagnetic with J =-0.27 cm?1, where the spin Hamitonian is defined as H =-2∑i,jJi,jSiS within the complex. 相似文献
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Ce1-xGdxO2-x/2的溶胶-凝胶法合成及其性质 总被引:14,自引:0,他引:14
利用溶胶-凝胶法合成了Ce1-xGdxO2-x/2(x=0.1~0.6)系列固体电解质, 系统地研究了其结构、热膨胀系数和导电性. XRD结果表明, 160 ℃即完全形成立方萤石结构. 由于溶胶-凝胶法合成的物质粒度均匀, 颗粒小, 故在较低温度(1 300 ℃)时即可形成高致密样品, 此温度明显低于传统的高温固相法烧结温度(1 600~1 650 ℃). 高温X射线衍射测得Ce0.8Gd0.2O1.9的热膨胀系数为8.125×10-6 K-1. 阻抗谱表明, 溶胶-凝胶法合成可减少或消除固体电解质的晶界电阻, 600 ℃时Ce0.8Gd0.2O1.9的电导率为5.26×10-3 S/cm, 活化能Ea=0.82 eV. 相似文献
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BaCe1—xRExO3—0.5x的溶胶—凝胶法合成及离子导电性 总被引:3,自引:0,他引:3
用溶胶-凝胶法合成了系列钙钛矿结构的BaCe1-xRExO3-0.5x(RE=La,Nd,Sm,Eu,Gd,Dy,Ho,Er和Y)复合氧化物,通过XRD和热分析对样品结构及生成过程进行了研究.测定了不同温度下样品的交流阻抗谱,讨论了稀土离子掺杂对BaCeO3电性质的影响.溶胶-凝胶法比固相反应法合成温度降低了600~800℃,稀土掺杂使BaCeO3离子导电率提高了10~40倍. 相似文献
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溶胶-凝胶法制备小颗粒(Y,Gd)BO_3∶Eu及其表征 总被引:1,自引:0,他引:1
用溶胶 凝胶方法制备了平均粒径为 1~ 2 μm的小颗粒、高发射效率的 (Y ,Gd)BO3 ∶Eu红色发射荧光体。用XRD、SEM、粒度分析和PL光谱对荧光体作了表征和研究。常规固相反应合成 (Y ,Gd)BO3 ∶Eu需在 1 2 0 0℃以上才能形成均一的固溶体。而溶胶 凝胶法制取稀土正硼酸盐 80 0℃灼烧已可形成均一的单相 (Y ,Gd)BO3 ∶Eu,在 1 1 0 0℃可得到发光亮度最高的荧光体。它的亮度是常规固相反应于 1 2 0 0℃制得的荧光体的 1 2 0 %。采用溶胶 凝胶法制取 (Y ,Gd)BO3 ∶Eu荧光体 ,可在相当宽的实验条件范围内得到小粒径、窄分布和高亮度的荧光体 ,且有良好的颗粒形貌。 相似文献
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