Solvothermal Synthesis,Crystal Structure,and Strong Luminescence of the First Organic‐Templated Europium Sulfate Chloride

The first organic amine templated europium sulfate chloride [C₆N₄H₂₂]_0.5Cl[Eu(SO₄)₂ · H₂O] ( 1 ) was synthesized solvothermally and structurally characterized by single‐crystal X‐ray diffraction, IR spectroscopy, TGA, and ICP. Crystal analyses of compound 1 shows a novel inorganic layer constructed from [–Eu–O–S–O–]_n chains. The adjacent chains are connected by sharing the bridging SO₄^2– groups to generate eight‐membered rings. The very strong luminescence in the red light region indicates compound 1 is an excellent candidate for red fluorescent materials.     

Solvothermal Synthesis,Crystal Structure,and Photocatalytic H2 Evolution of two CuII Coordination Polymers Based on Keggin Polyoxotungstates

Two new Cu^II coordination polymers based on α‐Keggin polyoxotungstates, [Cu₂(dpa)₂(H₂O)₂(GeW₁₂O₄₀)] · 0.5CH₃COOH ( 1 ) and [Hdpa][Cu₂(dpa)₂(4,4′‐bipy)(H₂O)₂(PW₁₀V₂O₄₀)] ( 2 ) (dpa = 2,2′‐dipyridylamine, 4,4′‐bipy = 4,4′‐bipyridine), were obtained by solvothermal reactions in glacial acetic acid and characterized by elemental analysis, IR spectroscopy, TG analysis, X‐ray powder diffraction, and single‐crystal X‐ray diffraction. Compound 1 exhibits a 1D two‐rowed chain constructed from [GeW₁₂O₄₀]^4– anions coordinated with [Cu(1)(dpa)]²⁺ and [Cu(2)(dpa)(H₂O)₂]²⁺ fragments by four terminal oxygen atoms. Compound 2 exhibits a 2D layered structure constructed from [PW₁₀V₂O₄₀]^5– anions coordinated with [Cu(dpa)(4,4′‐bipy)_0.5(H₂O)]²⁺ fragments by four terminal oxygen atoms. Furthermore, the electrochemical properties of 1 and the photocatalytic hydrogen production of 1 and 2 were investigated.     

单分散磁性纳米粒子固定化猪胰脂肪酶的研究

借助溶热法制备了一种亲水及生物相容良好的Fe3O4磁性纳米粒子,用γ-氨丙基三乙氧基硅烷直接对所得磁性粒子表面改性,然后用戊二醛偶联法制得了固定化猪胰脂肪酶.表征研究显示,所得磁性粒子粒径约200 nm,具有良好的单分散性和磁响应性.考察了戊二醛浓度、给酶量和反应时间对脂肪酶固定化过程的影响,并通过游离酶与固定化酶的比...     

溶剂热法制备Ag/TiO2纳米材料及其光催化性能

以乙醇为溶剂, 钛酸四丁酯为前驱体, 用溶剂热法制备了Ag表面修饰的负载型纳米二氧化钛光催化剂. 利用X射线衍射(XRD)、N₂吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、紫外-可见(UV-Vis)光谱等技术对其进行了系统的表征, 以亚甲基蓝(MB)溶液的脱色降解为模型反应, 考察了不同Ag含量样品的光催化性能. 结果表明: 用溶剂热法制备的样品中TiO₂皆为锐钛矿相, 金属Ag颗粒沉积在TiO₂表面, 粒径为2 nm左右, 比表面积较溶胶凝胶法制备的样品大大增加, 最高可达151.44 m²·g^-1; UV-Vis光谱和光催化实验表明: Ag修饰使TiO₂对光的吸收能力大大增强, 吸收带边红移至可见光区, 亚甲基蓝在该复合材料上的光催化降解反应遵循一级反应动力学模型; 溶剂热法制备样品的光催化性能明显好于溶胶凝胶法制备的样品, 在紫外光和可见光下, Ag摩尔分数为5%的样品表现出最佳的光催化活性.     

三维配位聚合物[Sr(BDC)(H2O)]的合成、结构与热稳定性

利用溶剂热法在硝酸锶、1,4-对苯二甲酸（BDC）、N,N′-二甲基甲酰胺（DMF）和水体系中合成了一种新的配位聚合物[Sr（BDC）（H₂O）]（1）,并通过单晶X射线衍射、变温粉末X射线衍射、元素分析、红外光谱和热重-质谱联用对其进行了表征.该化合物属正交晶系的Pbca空间群,晶胞参数为a=1.1854（2）nm,b=0.7122（1）nm,c=2.0031（4）nm.该化合物具有三维网络结构,由共面的SrO₈四方反棱柱组成的zigzag链通过1,4-对苯二甲酸配体连接而成.热重-质谱联用和变温粉末X射线衍射分析表明它的骨架具有较高的热稳定性。     

Synthesis of Mn-doped ZnO diluted magnetic semiconductors in the presence of ethyl acetoacetate under solvothermal conditions

Mn-doped ZnO samples with 5%, 20% and 40% nominal Mn concentrations were prepared in the presence of ethyl acetoacetate under solvothermal conditions. UV absorption spectroscopic analysis discloses that chemical modification was achieved by reaction of Zn or Mn precursor with ethyl acetoacetate in ethanol medium. XRD and HRTEM characterizations indicate that ZnMnO₃ impurity phase was formed in the 20% and 40% Mn-doped ZnO samples while no secondary phase was present in the 5% Mn-doped sample. The 5% Mn-doped sample consists of spheroid-like particles with size of 10-50 nm and has a real Mn concentration of 3.2%. Ferromagnetism and paramagnetism coexist in the 5% Mn-doped ZnO sample at room-temperature, which may arise from ferromagnetic exchange interaction as well as small secondary phases. The 20% and 40% Mn-doped samples show large paramagnetic effects at room temperature. Small paramagnetic secondary phases and clustering of Mn are probably responsible for this.     

[M(en)3]2Sn2Se6(M=Mn,Zn)的制备及其热稳定性

用有机溶剂热生长技术(SolvothermalTechnique)制备过渡金属锰和锌硒化物[Mn(en)3]2Sn2Se6(Ⅰ),[Zn(en)3]2Sn2Se6(Ⅱ).用单晶X射线衍射技术对其进行晶体结构分析.[Zn(en)3]2Sn2Se6样品的热分析结果表明,该化合物的热分解分三步进行.光学性质测试表明它们是半导体材料,[Mn(en)3]2Sn2Se6的能带隙为1.76eV.[Zn(en)3]2Sn2Se6的能带隙为2.49eV.     

单晶BaTiO3纳米线的低温溶剂热法制备和表征

采用溶剂热技术,以有机钛偶合体胶束作模板成功制备了立方相单晶钛酸钡纳米线,并通过X射线衍射(XRD)、能量损失谱(EDX)、透射电子显微镜(TEM)、高分辨电子显微镜(HRTEM)、选区电子衍射(SAED)对钛酸钡纳米线进行了表征。钛酸钡纳米线呈均匀的直线形,直径为20～60nm,长度达到十几微米。并对BaTiO3纳米线的形成机理进行了浅析。     

Synthesis,Crystal Structure,Optical, Magnetic,and Thermal Properties of the New Heteroleptic Chromium Complex [Ph4P][Cr(en)(S5)2]

The new heteroleptic chromium complex [Ph₄P][Cr(en)(S₅)₂] has been synthesised under mild solvothermal conditions by the reaction of chromium trichloride, sulfur, and tetraphenylphosphoniumbromide in a solution of ethylendiamine ( en ) in water. The crystal structure consists of isolated tetraphenylphosphonium cations and [Cr(en)(S₅)₂]^– anions. The Cr³⁺ cations are in an octahedral coordination of two bidentate S₅^2– polysulfide anions and one bidentate en ligand. The N atoms of the en ligand and the terminal S atoms of the S₅^2– anions bonded to the Cr³⁺ ions are in a cis-position. The six-membered CrS₅ rings are in a chair conformation. The three dimensional arrangement of the cations and anions is achieved via intermolecular hydrogen bonds. Investigations with differential thermal analysis (DTA) combined with thermogravimetry (TG) show a stepwise decomposition. In the first step the en ligand is removed completely followed by the emission of a part of the tetraphenylphosphonium cations and the sulfur atoms in the second step. The temperature dependence of the magnetic susceptibility exhibits a Curie-Weiss behaviour with an effective magnetic moment typical for a Cr³⁺ (d³) ion and a value for the Weiss constant of 1.3(2) K. Fourier transform infrared spectroscopy (FTIR) was also performed to characterise the optical properties.     

Influence of pH variation on structural,optical, and superparamagnetic behavior of Ni-doped ZnO (X=0.02) using a solvothermal method

Zn1-xNixO nanoparticles at a concentration (2%) with pH variation (4, 5, 8 and 9) are successfully synthesized using the solvothermal method. ZnO nanoparticle has a hexagonal wurtzite structure when synthesized at acidic and basic conditions. In pH, the solution is calculated from 4 to 9 by the composed addition of NaOH and HCl. The structural properties are studied from XRD and TEM. The average particle size is found to be 13.2 nm using the Debye Scherrer formula and optical properties are analyzed through UV–Visible, FTIR, & PL. From the absorption spectra, it is observed that the bandgap energy is inversely proportional to the particle size. UV–Vis and PL are used to study the optical behavior of the samples. The magnetic behavior of Zn1-xNixO exhibit changing behavior from paramagnetic to superparamagnetic structure with increases in their pH values.