Ba2SbInO6双钙钛矿的水热合成和表征

利用水热晶化法制备了Ba₂SbInO₆纯相，并通过XRD、SEM、IR、XPS和ICP等方法，对产物的物相、形貌、结构和组成进行了表征。初步结构表征结果表明，产物可能为B位离子无序排列的立方钙钛矿结构，空间群为Pm3m，晶胞参数为a=0.4132 mm。产物粉末呈现立方晶型，粒度约为0.5～2 μm。     

Ba2InSbO6双钙钛矿的水热合成及 121Sb M?ssbauer谱表征

在温和水热条件下,合成了双钙钛矿型Ba₂InSbO₆,采用XRD、TEM、XPS、ICP及IR等技术表征产物的结构及组成。XRD数据的Rietveld拟合结果表明,Ba₂InSbO₆为a=0.416 782(13) nm的立方钙钛矿结构,属于Pm3m。 ¹²¹Sb M?ssbauer谱测试表明,产物的同质异能移可归属为Sb^Ⅴ及Sb-O键具有明显的共价特征。合成条件的研究表明,Sb源对合成具有重要影响,且Sb₂O₃锑源可有效地降低杂质的生成。     

掺杂型稀土双钙钛矿光催化剂La2FeTiO6葡萄糖络合法制备与表征

采用葡萄糖络合法制备了双钙钛矿型催化剂La2FeTiO6,进行不同量Sr掺杂改性。利用X射线粉末衍射(XRD)、H2-程序升温还原(H2-TPR)、比表面(BET)、扫描电镜(SEM)、磁性与电性测试等手段对其进行表征,以可见光催化降解对氯苯酚为探针讨论了Sr掺杂对La2FeTiO6催化剂的物理化学性质及可见光催化活性的影响。结果表明:催化剂La2FeTiO6在掺杂Sr后,催化剂的可见光催化活性均有所提高,其中Sr掺杂量为0.08时,催化剂的光催化活性提高最大,光照1 h时对氯苯酚的降解率就已经达到了90%,5 h后降解率达到99.2%。La2FeTiO6通过Sr掺杂改性后光照5 h降解率提高了37.1%。比表面测试和程序升温还原试验结果表明,碱土金属Sr的掺杂提高了催化剂的比表面,促进了双钙钛矿La2FeTiO6中Fe的还原,使其还原峰面积增大,还原温度也有所降低。电性和磁性测量结果说明,碱土金属Sr的掺杂明显影响其催化剂的电磁性能。     

钒磷酸盐(NH3CH2CH2NH2)[VOPO4]的水热合成和结构表征

标题化合物是在反应物摩尔比为V₂O₅∶H₃PO₄∶H₂NCH₂CH₂NH₂∶H₂O＝0.55∶4∶3.6∶265时, 175 ℃水热反应5 d合成的. 其结构特点是: 钒八面体[VO₅N]共用角顶的氧形成“之”字型链, 链间由[PO₄]共角顶连接成层; 乙二胺分子的一个N直接与V配位, 并伸向层间. 相邻层间存在强氢键. 晶体学数据: 单斜晶系, P2₁/c (No. 14), a＝0.92108(2) nm, b＝0.72851(1) nm, c＝0.98204(2) nm, β＝101.269(7)°, V＝0.6462(4) nm³, Z＝4, D_c＝2.303 g•cm^－3, R₁＝0.0417, wR₂＝0.0999.     

[C6N2H18]2[Mo5O15(HPO4)2]·H2O的水热合成与结构表征

通过水热法合成了一个新化合物[C6N2H18]2[Mo5O15(HPO4)2]·H2O,并通过IR光谱、ICP、元素分析、差热与热重分析和X射线单晶衍射分析等手段进行了表征.结果表明,晶体属三方晶系,P3(2)21空间群,a=1.1231(1)nm,c=2.2802(5)nm,V=2.4911(7)nm3,Dx=2.835Mg/m3,Z=6,最后的一致性因子R=0.0227,wR=0.0675.阴离子中Mo5O15构成一环状结构,2个HPO4一个连在环的下方,一个连在环的上方,形成类似于“飞碟”状的结构,阳离子为2个质子化的四甲基乙二胺.     

Mn位掺杂钙钛矿结构化合物LaSr2Mn2-xNixO7的磁性和电性的研究

The effect of Ni substitution for Mn on magnetic and transport properties has been investigated for layered manganese oxides LaSr₂Mn_2-xNi_xO₇. Nickel doping hampered the canted antiferromagnetic (AFM) exchange at low temperature and their Neel temperature (T_N) decreased from 138 K (x=0) to 102 K (x=0.3). Meanwhile, spin glass, charge ordering and metal-insulator transition are suppressed by Ni addition. The resistivity increases obviously with increasing x due to double exchange interaction channel broken by Ni²⁺ addition. The resistivity of all samples in low temperature range fits to the Mott′s variable rang hopping (VRH) model, while it fits to nearest neighbor hopping of small polarons model in high temperature range.     

AgNbO3的水热合成和光催化性质表征

采用水热合成法制备了AgNbO3粉末,运用XRD(X-ray diffraction),SEM(Scanning Electron Microscope)和UV Vis DRS (diffuse reflectance spectroscopy)对其表征,在可见光照射下通过降解亚甲基蓝,来评估样品的光催化活性,实验结果表明,目标化合物与固相合成法制备的AgNbO3相比较具有明显较高的催化活性,水热法制备的产物在光催化方面拥有广阔的应用前景.     

AaZrO3基质固体电解质的水热合成与表征

利用水热晶化法制备了ＢａＺｒＯ３纯相和ＢａＺｒ１－ｘＭｘＯ３－ａ（Ｍ＝Ａｌ，Ｇａ，Ｉｎ；ｘ≤０．２０）体系固体电解质通过ＸＲＤ，ＳＥＭ，ＩＲ，＾２７ＡｌＭＡＳＮＭＲ和化学分析，对产物的物相，粒度和掺杂质进入晶格的数量进行了表征。     

Na2SO4辅助水热合成SnO2纳米晶

系统地研究了以SnCl₄·5H₂O为原料，以Na₂SO₄为矿化剂，采用水热法在较低温度下和较短的反应时间内制备结晶良好并均匀分散的SnO₂纳米晶。采用X射线衍射(XRD)、透射电子显微镜(TEM)、红外光谱(IR)等技术对水热反应的晶化过程进行了分析。结果表明：在Na₂SO₄存在的情况下，在120 ℃反应4 h 即可制备得到晶粒细小，分散性能良好的SnO₂纳米晶。XRD衍射峰峰宽随水热温度的升高或反应时间的延长而变窄，结晶性提高。TEM结果表明产物颗粒小、分散性能良好。水热反应温度和反应时间对产物结晶度和粒径有明显的影响。对Na₂SO₄在反应过程中的作用机理进行了分析。     

Hydrothermal Synthesis and Dielectric Characterization of a Double Perovskite Ba2FeSbO6

A double perovskite oxide Ba₂FeSbO₆ was hydrothermally synthesized and structurally characterized by X-ray diffraction. This solid compound shows a single phase and has a trigonal structure with space group R m and cell parameters of a=0.57261 nm and c=1.40244 nm. The dielectric constant and loss tangent of the solid measured in a frequency range from 100 Hz to 1 MHz at temperatures from 313 K to 513 K reveal a relaxation process of frequency dependence of the real part(ε') of dielectric constant and dielectric loss tand. The frequency dependence of electrical property led to the framework of conductivity and electric modulus formalisms. The scaling behavior of imaginary part of electric modulus suggests that the relaxation describes the single mechanism at various temperatures. The variation tendency of the alternating current impedance indicates the thermally activated conduction process follows Jonsche’s power law.     

Hydrothermal Synthesis,Structure Characterization and Magnetic Studies of Perovskite-type Fluorides K2NaVF6 and (NH4)aVF6

Two perovskite-type fluorides K2NaVF6 and (NH4)3VF6 were synthesized under mild hydrothermal conditions.The structures of the compounds were determined by means of powder X-ray diffraction analysis.The...     

Hydrothermal Synthesis,Structure and Characterization of a New 2D Co(II) Coordination Polymer Based on Flexible Double Imidazole Derivative and Oxalate

A 1D supramolecular compound [dmbbbi](1) and a 2D cobalt coordination polymer [Co(dmbbbi)(ox)]₂(2) [dmbbbi=1,1-(1,4-butanediyl)bis(5,6-dimethylbenzimidazole), ox=oxalate], C₄₈H₅₂Co₂N₈O₈, were obtained under hydrothermal conditions by tuning the molar ratio of the reactants. The crystal structure analysis reveals that in compound 1, the adjacent dmbbbi molecules connect with each other via hydrogen bonds to form a 1D supramolecular chain. In compound 2, two crystallographically independent Co²⁺ ions show the same six-coordination mode. Each Co²⁺ ion is coordinated by four oxygen atoms from two ox anions and two nitrogen atoms from two cis-dmbbbi ligands. The adjacent Co²⁺ ions are bridged by ox anions to generate an infinite 1D zigzag chain, which is extended by pairs of dmbbbi ligands to form a 2D honeycomb-like (6,3) network. Moreover, the thermal stability and the electrochemical property of compound 2 were studied.     

Hydrothermal Synthesis and Characterization of Perovskite Oxide AgTaO3

The perovskite-type AgTaO₃ crystals were prepared by mild hydrothermal method and determined by powder X-ray diffraction. Rietveld refinement indicates that AgTaO₃ crystallized in an orthorhombic system with the space group Pcmn. The lattice parameters are a=5.5822(1) nm, b=7.8522(2) nm and c=5.5347(1) nm, with α=β=γ= 90.0o. The compound was characterized by scanning electron microscopy(SEM), X-ray photoelectron spectroscopy (XPS), high resolution transmission electron microscopy(HR-TEM) and UV-Vis diffuse reflectance spectrometry (UV-Vis DRS). The photocatalytic activity of AgTaO₃ powder was evaluated by the degradation of Congo red under UV-light irradiation. The result shows that the titled compound has a high photocatalytic activity at room temperature and potential application in photocatalysis.     

Ba2InSbO6双钙钛矿的水热合成及121Sb M(o)ssbauer谱表征

在温和水热条件下,合成了双钙钛矿型Ba2InSbO6,采用XRD、TEM、XPS、ICP及IR等技术表征产物的结构及组成.XRD数据的Rietveld拟合结果表明,Ba2InSbO6为a=0.416782(13)nm的立方钙钛矿结构,属于Pm-3m.121Sb M(o)ssbauer谱测试表明,产物的同质异能移可归属为SbV及Sb-O键具有明显的共价特征.合成条件的研究表明,Sb源对合成具有重要影响,且Sb2O3锑源可有效地降低杂质的生成.     

液固相水热法制备氧化硅纳米线

利用液固相水热反应方法, 以硅溶胶为硅源, 在三价铁辅助下与乙二胺的水溶液在180 ℃反应4 d后生成具有P21212空间群结构的单晶氧化硅纳米线. 用扫描电子显微镜、透射电子显微镜和多晶X射线衍射对制备的样品进行了表征, 系统研究了有机胺、金属盐、反应时间及反应温度等条件对氧化硅纳米线生长的影响. 结果表明, 随着有机胺碳链的增长, 产物形貌逐渐由纳米线转变为纳米片; 金属阳离子的存在对纳米线形貌有较大的影响, 而阴离子的存在并不影响纳米线的生成; 过低的铁含量导致反应进行不完全, 而过多的铁盐加入则会导致反应中剩余铁氧化物吸附到氧化硅纳米线表面, 进而影响到产物纯度; 反应时间延长及反应温度的提高都有利于氧化硅纳米线的生长. 最佳反应条件为: 有机胺为乙二胺, 硝酸铁为铁源, 硅溶胶为硅源, 硅/铁摩尔比为1∶0.4, 乙二胺与水的体积比为8∶5, 温度为180 ℃.     

水热法制备聚苯胺及其铁氧化物纳米复合材料

利用水热法与无模板自组装法相结合, 以三氯化铁为氧化剂、 掺杂剂和反应物, 制备了聚苯胺及其铁氧化物纳米复合材料. 结果表明, 通过改变三氯化铁的浓度可以调控产物的微观结构和组成. 当三氯化铁的浓度≤0.13 mol/L时, 产物组成为未掺杂的低聚苯胺与α-Fe₂O₃的复合纳米材料, 其微观结构为纳米颗粒组装成的椭球体和准立方体; 当三氯化铁的浓度≥0.20 mol/L时, 产物组成为掺杂态聚苯胺, 其微观结构为纳米片层结构组装成的微米级大丽花球; 并且产物的粒径随三氯化铁浓度的增大而增大. 利用扫描电子显微镜、 红外光谱、 紫外-可见光谱、 X光电子能谱及X射线衍射等手段对产物的微观结构和组成进行了表征, 并探讨了产物的形成机理.     

新型化合物[Ni(en)2V6O14]n的水热合成与晶体结构

金属 -氧簇合物在催化吸附、医药临床、能量存储和材料科学等方面的应用越来越受到关注 [1～ 3 ] .钒 -氧簇合物的结构新颖 ,在材料领域中具有广泛的应用前景 .采用水热合成技术 ,以简单的无机、有机起始原料在相对低温下制备金属 -氧簇合物晶体是近年来刚刚兴起的研究工作 [4 ] ,并且已经合成出一维链状化合物 Cu(prn) 2 V2 O6[5]、层状结构 Ni(C10 H8N2 ) 2 V3 O8.5[6]及三维网状结构 (H2 en Me)[Ni(en) 2 V12 O2 8][7] .我们采用水热技术合成了由 { V V 2 O7} n 单元层与桥配体 [Ni(en) 2 ]2 +构建的三维无机 -有机化合物 [Ni(en…     

Hydrothermal Synthesis, Structural Characterization and Properties of Mixed Valent Decavanadium Oxide [Co_2Cl_8V_(10) O_(18)(H_2O)]Cl_2·6H_2O with Novel Three-dimensional Framework

IntroductionPolyoxometalates constitute an enormous classof compounds whose unusual versatility and reac-tivity afford practical applications to many fields,such as catalysis,biology,medicine,and materialsciences[1— 4] .In recent years,hydrothermal tech-nique has become a vital tool in self- assemblychemistry.This technique,in combination with or-ganic templates,has been demonstrated to be wellsuited for the synthesis and the crystal growth ofpolyoxometalates with novel structures[5— 9] .Amo…     

新型三维结构亚磷酸钒(Ⅲ)[V2(HPO3)3·(H2O)3]·H2O的水热合成与晶体结构

在具有开放骨架结构的过渡金属磷酸盐微孔材料的合成中，钒磷酸盐因在催化和磁学方面具有潜在的性质和特殊结构特征而引起人们的广泛兴趣．近年来，人们正在尝试用假四面体结构的[HPO3]^2-替代四面体结构的[PO4]^3-，因为{HPO3}结构基元同钒原子的连接方式与{PO4}结构基元和钒原子的连接方式具有明显的差别，