Hydrothermal Synthesis and Structure Characterization of Compound Zn（Hpydc）2（H2O）（pydc=pyridine—2,5—dicarboxylate）

1 INTRODUCTION The researches in zinc complexes have been rapidly expanding because of their fascinating structural diversity and potential applications as functional materials and bioloenzymes[1~5]. A lot of compounds of different structural types containing zinc metal have been synthesized and reported[6~9]. In these complexes, the multifunction ligand, such as polyamine, polyacid, and so on, were often elected. In order to obtain more compounds having novel structures, recently, we ch…     

Hydrothermal Synthesis and Crystal Structure of a New Hexa-cobalt-containing POM

A new compound Na3H3[Co（en）3]2[Co4（H2O）2（PW9O34）2]·11H2O 1 （en = ethylenediamine） has been synthesized under hydrothermal conditions and characterized by IR, TGA, and single-crystal X-ray diffraction analysis. Crystal data： monoclinic, space group C21c, a = 26.336（5）, b = 18.135（2）, c = 22.751（4）A, β = 123.039（7）° and Z = 4. X-ray crystallographic study on compound 1 reveals that it includes a Weakley-type sandwich polyoxoanion [Co4（H2O）2（PW9O34）2]^10-, two complex ions [Co（en）3]^2＋, three Na^＋ ions （one Na（1） and two Na（2））, and eleven crystallographic water molecules. The sandwich polyoxoanions are linked by Na2 to form 2D layers parallel to the （100） plane, and these layers are further connected by Nal along the α-axis to generate a 3D structure.     

Hydrothermal Synthesis,Crystal Structure and Magnetic Property of a New Co（Ⅱ） Complex：[Co（4,4＇-bpy）_2（H_2O）_2（4-FBA）_2]·（4,4＇-bpy）

A new complex [Co(4,4'-bpy)2(H2O)2(4-FBA)2]·(4,4'-bpy)(1) has been hydro-thermally synthesized using cobalt,4,4'-bipyridyl(4,4'-bpy) and 4-fluorobenzoic acid(4-HFBA),and characterized by thermal analysis,single-crystal X-ray diffraction and magnetic property.The complex crystallizes in the triclinic system,space group P,Z = 1.Crystal data:C54H44CoF2N8O6,Mr = 997.90,a = 9.134(2),b = 11.555(2),c = 12.867(3) ,α = 66.02(3),β = 77.96(3),= 73.11(3)°,V = 1180.9(4) 3,Dc = 1.403 g/cm3,μ(MoKα) = 0.433 mm-1,F(000) = 517,the final R = 0.0633 and wR = 0.1171 for 2152 observed reflections(I > 2σ(I)).The title complex is assembled into 1D supramolecular chains parallel to [001] based on the adjacent molecular ··· stacking interactions and hydrogen bonds.The variable temperature magnetic measurements show a weak ferromagnetic behavior over 300-160 K followed by antiferromagnetic behavior below 160 K for the title complex.     

水热法合成SnO2金红相纳米柱和亚微米晶体

本文采用水热法,以SnCl4·5H2O为前驱物,在180℃,填充度为68;,反应时间8h,强酸环境条件下合成了SnO2纳米金红相晶体,直径约为5～10nm,长30～100nm.加入一定量的NaOH,调节溶液pH值为强碱性(pH=11),同样条件下也合成了SnO2金红相纳米柱晶体,长200nm、直径10～20nm.提高水热反应的温度为430℃,矿化剂为3mol/L NaOH,反应时间24h,合成了亚微米金红相SnO2晶体,最大线度为300nm.     

表面活性剂对水热合成Gd2O3∶Eu3+性能的影响

以碳酸氢铵作为沉淀剂,分别以聚乙二醇-1000(PEG-1000)、十二烷基磺酸钠(DSASS)、十六烷基三甲基溴化铵( CTAB)、乙二醇(EG)为表面活性剂,采用水热法制得了棒状Gd2O3∶ Eu3+微晶.用XRD、SEM、荧光光谱仪等分别对样品的物相结构、微观形貌和发光性能进行了研究.结果表明:采用不同的表面活性剂所得前驱物经800℃下焙烧均得到了纯立方相的Gd2 O3∶Eu3+微晶,颗粒基本呈棒状,分散性较好,但长径比不同.以PEG-1000为表面活性剂所得样品尺寸不均一,尺寸分布范围较宽;以DSASS、CTAB、EG为表面活性剂所得样品直径较小、长度较短,且尺寸分布范围较窄.棒状Gd2O3∶Eu3+微晶主发射峰位置均在613 nm,属于5D0→7F2跃迁,呈红光发射;激发光谱中电荷迁移态发生了红移,主激发峰位于261nm.表面活性剂种类对发射峰和激发峰强度影响较大,由强到弱的顺序为:PEG-1000＞ DSASS＞ CTAB＞ EG.     

Ni(phen)(H2O)(V2O6)的水热合成和晶体结构（英）

A novel compound Ni(phen)(H₂O)(V₂O₆) has been hydrothermally synthesized and structurally determined to be a two-dimensional compound, which contains {V₂O₆}_n^2n- chains interconnected by nickel(Ⅱ) complexes via oxygen atoms. The crystallographic data measured by single-crystal X-ray diffraction analysis are as follows: C₁₂H₁₀N₂NiO₇V₂, M_r=454.81, monoclinic, space group P2₁/c, a=0.784 6(3), b=2.103 6(8), c=0.942 3(4) nm, β=112.872(5)°, V=1.433 0(10) nm³, Z=4, D_c=2.104 Mg·m^-3, μ(Mo Kα)=2.615 mm^-1, F(000)=904, T=298(2) K, 4 480 reflections collected, 2 470 independent (R_int=0.032 2), the final R=0.058 4 and wR₂=0.145 7 for 2 303 observed reflections with I>2σ(I). CCDC: 192520.     

硝酸根离子介质中偏钛酸钡的水热合成

以硝酸和钛酸四丁酯为原料，在２４０℃的碱液中成功地制备了四方相ＢａＴｉＯ３运用ＸＲＤ、ＤＳＣ和ＩＲ等技术碱度、硝酸根离子、钛源活性、填充度等因素对ＢａＴｉＯ３形成、粒度和物相的作用，ＫＯＨ最适宜浓度为１．０ｍｏｌ／Ｌ，碱液中ＢａＴｉＯ３是ＢａＯ－ＴｉＯ２体系中最稳定的物相，硝酸根离子参与了ＢａＴｉＯ３晶体的成核和生长，钛源的高活性和高填充度有利于四方ＢａＴｉＯ３的形成。     

Keggin型配合物（C12H9N2）3[PMo12O40]的水热合成及晶体结构

采用水热反应合成了有机-无机杂化的Keggin型配合物（C12H9N2）3[PMo12O40],并通过X-射线单晶衍射对其结构进行了分析。该配合物为正交晶系P212121空间群,晶胞参数为a=1.20800（1）nm,b=2.10108（4）nm,c=2.24234（5）nm。配合物包含了孤立的Keggin型[PMo1...     

丙三醇辅助水热法合成纳米棒状LiFePO4

在丙三醇存在下,以FeSO4·7H2O,LiOH·H2O和H3 PO4为原料,采用水热法合成了橄榄石结构的纳米棒状LiFePO4.产物结构与形貌用X射线衍射、红外、扫描电子显微镜、能谱分析测试技术进行了表征.讨论了反应时间、温度、混合溶剂比例对产品形貌的影响.结果表明,当V(水)/以丙三醇)=2:1时,在180℃反应2...