RESr2RuCu2O8(RE=Gd和Eu)的合成与物性研究

报道了磁性超导体RESr2RuCu2O8(RE=Gd和Eu)单相样品的合成以及对其结构和物性的研究。结果表明，这类化合物的结构和YBa2Cu3O7-δ相类似；在这两类化合物中，超导电性与弱铁磁有序共存；两样品铁磁相变温度TM分别为136，130K，超导临界温度TC分别为46，35K；由于Gd^3 和Eu^3 离子磁矩的不同，两样品的磁性质存在一定的差别。     

La2M2O7(M=Ti,Zr)多晶粉末的低温水热合成及表征

低温水热合成是水热化学一个活跃的研究方向,在氧化物粉末的合成方面具有潜在的应用价值.La2M2O7(M=Ti,Zr)陶瓷材料的优良特性使其多晶粉末的合成倍受关注[1,2].     

Co(μ2-bpy)V2O6(bpy=4,4′-联吡啶)的水热合成和晶体结构

采用CoCl2·6H2O、4,4′-联吡啶和NH4VO3,以H2O作溶剂(摩尔比1:2:2:1950)在170℃下水热反应合成无机-有机杂化化合物Co(μ2-bpy)V2O6(bpy=4,4′-联吡啶),经单晶X射线衍射测定其晶体结构.此晶体属三斜晶系,空间群为Pi,晶胞常数a=0.81599(7)nm,b=0.85826(7)nm,c=1.02031(8)nm,α=87.111(2)°,β=75.305(2)°,y=74.784(2)°,Z=2.Co(μ2-bpy)V2O6是无机的双金属氧化物层,[Co2V4O12]n通过有机的桥式配体μ2-bpy以N-Co配位键桥联而成.晶体的三维共价结构含有多种开放式孔道,其中最大孔道的尺寸为0.5nm×0.7nm.漫反射光谱研究表明,此晶体具有约2.0 eV的光学能隙,属于半导体,在420℃以下是热稳定的.     

Co(μ2-bpy)V2O6 (bpy =4,4′-联吡啶)的水热合成和晶体结构

采用CoCl2•6H2O、4,4′-联吡啶和NH4VO3,以H2O作溶剂（摩尔比1∶2∶2∶1950）在170 ℃下水热反应合成无机-有机杂化化合物Co(μ2-bpy)V2O6 (bpy=4,4′-联吡啶), 经单晶X射线衍射测定其晶体结构.此晶体属三斜晶系,空间群为Pī,晶胞常数a=0.81599(7) nm,b=0.85826(7) nm, c=1.02031(8) nm,α=87.111(2)°, β=75.305(2)°,γ=74.784(2)°, Z=2. Co(μ2-bpy)V2O6是无机的双金属氧化物层,[Co2V4O12]n通过有机的桥式配体μ2-bpy以N－Co配位键桥联而成.晶体的三维共价结构含有多种开放式孔道,其中最大孔道的尺寸为0.5 nm×0.7 nm.漫反射光谱研究表明,此晶体具有约2.0 eV的光学能隙,属于半导体,在420 ℃以下是热稳定的.     

γ—Mo2N合成过程中的热变化及中间产物的研究

采用ＤＴＡ技术，通过改变升温速率研究了γ－Ｍｏ２Ｎ合成过程中的热变化，并经ＸＲＤ，ＢＥＴ及ＩＲ测试，对ＤＴＡ曲线中的谱峰进行归属，考察了中间产物，ＤＴＡ结果表明，在ＭｏＯ３和ＮＨ３程序升温反应过程中有放热峰及吸热峰出现，且随升温速率的长高，放热峰面积与吸热峰面积之比逐渐减小，结合ＸＲＤ及ＩＲ结果可知，ＤＴＡ曲线听放热峰可归属为由ＭｏＯ３变化为ＭｏＯ２的还原峰，吸热峰则归属为由ＭｏＯ２变化为Ｍｏ２Ｎ     

[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构

氯化钆;甘氨酸;固态配合物;[Gd(Gly)3(H2O)2]Cl3·H2O的合成与晶体结构     

固相法合成锂离子电池正极材料LiMn2O4

用Li2CO3和Min(OAc)2@4H2O为锂锰源,添加少量柠檬酸或草酸在550℃煅烧4h合成了尖晶石LiMn2O4.采用X-射线衍射法,透射电镜和充放电测量研究了它们的结构和性质.用Scherre公式计算样品粒度在28.5nm～40.0nm.添加草酸制备的样品充放电性能较好,首次充放电的放电容量可达115mAhg-1.     

原位XRD反应装置下H2O对Fe5 C2的物相及F-T反应性能影响的研究

将原位XRD反应装置与在线气相色谱技术结合,研究了不同H_2O含量(4.36%、1.68%、0.56%)条件下单一相Fe_5C_2的氧化速率,并考察了不同Fe_5C_2氧化程度(0、25%、55%、68%)和氧化次数对其费托合成(F-T)反应性能的影响。研究结果表明,Fe_5C_2物相的氧化速率随H_2O含量的提高而逐渐增加,同时H_2O氧化使Fe_5C_2颗粒粒径减小,暴露出更多活性位点,造成F-T反应活性提高,且氧化程度越大,活性提高越明显;随着氧化次数的增加,F-T反应活性逐渐提高,但CH_4选择性增加,C_(5+)选择性逐渐降低。     

金刚烷甲酸铜(Ⅱ)配合物Cu(ada)2(py)2(H2O)的合成和晶体结构

金刚烷甲酸铜(Ⅱ)配合物Cu(ada)2(py)2(H2O)的合成和晶体结构     

Phase Equilibria in the V2O5-Sb2O4 System

Differential thermal analysis (DTA) and X-ray powder diffraction (XRD) were used to study phase equilibria, established in air in the V₂O₅-Sb₂O₄ system up to 1000°C. It has been found that there is a new phase =SbVO₅. The =SbVO₅ has been prepared by two methods: by heating equimolar mixtures of V₂O₅ and α-Sb₂O₄ in air and by oxidation of the known phase of rutile type obtained in pure argon at temperatures between 550 and 650°C. Thermal decomposition of =SbVO₅ in the solid state starts at 710°C giving off oxygen. The results provide a basis for constructing only a part of the phase diagram of the investigated system (up to 50.00 mol% Sb₂O₄). This revised version was published online in July 2006 with corrections to the Cover Date.     

Phase relations in the system ZnV2O6 -ZnFe2O4

Using DTA and XRD methods, a diagram of phase equilibria in ZnV₂O₆-ZnFe₂O₄ system has been constructed. System ZnV₂O₆-ZnFe₂O₄ is in subsolidus area a real binary system and its components form a compound Zn₂FeV₃O₁₁. Zn₂FeV₃O₁₁ melts incongruently at 835±5°C with deposition of two solid phases: b-Zn₂V₂O₇ and ZnFe₂O₄. This revised version was published online in July 2006 with corrections to the Cover Date.     

Initial Studies on the Oxide System Cr2O3–Sb2O4

Differential thermal analysis (DTA) and X-ray diffraction (XRD) were utilized to study the phase equilibrium established in the subsolidus area of the system Cr₂ O₃ –Sb₂ O₄ . It was found that the components of the title system interact in ambient air to produce CrSbO₄ . The compound is stable up to ~1380°C, at which temperature it starts to decompose. This revised version was published online in August 2006 with corrections to the Cover Date.     

Combined DTA and XRD Study of Sintering Steps Towards YAl3(BO3)4

Sintering processes in the Y₂O₃–Al₂O₃–B₂ O₃ system and its subsystems (Y₂O₃–B₂O₃ and Al₂ O₃–B₂O₃) have been investigated by using combined DTA and XRD measurements to get a better understanding of solid state chemical changes resulting in the formation of yttrium aluminum borate (YAl₃(BO₃)₄, YAB) phase and to study the possible role and contribution of various simple borates formed also in the former processes. Two new exothermic heat effects of YBO₃ formation have been detected by DTA in the Y₂O₃–B₂O₃ system between 720 and 980°C. In the Al₂O₃–B₂O₃ system a new experimental XRD profile of Al₄B₂O₉ was observed. Formation of these borates seems to promote the nucleation of double borate YAB below 1000°C. Conversion of Al₄B₂O₉ to Al₁₈B₄ O₃₃ was observed after a long term (10 h) sintering at 1050°C. Similarly, an increased formation of YAB has been observed as a product of the sintering reaction between YBO₃ and Al₁₈B₄O₃₃ at 1150°C. The two latter single borates are found to be identical with the high temperature decomposition products of YAB. This revised version was published online in July 2006 with corrections to the Cover Date.     

Phase equilibria in the system NiO-V2O5-Fe2O3 in subsolidus area

Reactivity of FeVO₄ towards Ni₂V₂O₇ and Ni₃V₂O₈ in the solid state was investigated. On the base of XRD and DTA results, phase diagrams in subsolidus area of the FeVO₄-Ni₂V₂O₇ and FeVO₄-Ni₃V₂O₈ intersections of the ternary system NiO-V₂O₅-Fe₂O₃ have been worked out and the phase diagram of this ternary system in subsolidus area in the whole component concentration range has been verified. This revised version was published online in July 2006 with corrections to the Cover Date.     

Studies on the System ZnO-V2O5-Fe2O3 Reactivity of ZnFe2O4 Towards ZnV2O6

Studies on the reactivity of ZnFe₂O₄ towards ZnV₂O₆ revealed that in the solid state the phases interact in a molar ratio of 1:3 to form a new compound, to which the molecular formula Zn₂FeV₃O₁₁ was assigned. The compound melts congruently at 825±5°C. This revised version was published online in July 2006 with corrections to the Cover Date.     

Phase relations in subsolidus area of ZnO-V2O5-Fe2O3 system

Phase equilibria in subsolidus area in the ZnO-V₂O₅-Fe₂O₃ system have been investigated over the whole concentration range of the oxides. The components of this system form two compounds: Zn₂FeV₃O₁₁ and Zn₃Fe₄(VO₄)₆. A solidus area projection onto the component concentration triangle plane of the ZnO-V₂O₅-Fe₂O₃ system has been constructed using DTA and XRD methods. 11 subsidiary subsystems can be distinguished in this system. Melting temperatures of mixtures of solid phases coexisting at equilibrium in each of subsidiary subsystems were determined. This revised version was published online in July 2006 with corrections to the Cover Date.     

DTA,TG studies of catalytic oxidation of carbon particles over M2 III O3 (MIII=Al,Cr, Fe,Ni)

Carbonizate as a model soot has been submitted to oxidation using Al₂O₃, Cr₂O₃, Ni₂O₃ and Fe₂O₃ as catalysts in the temperature range from RT up to 1000°C. The results obtained indicate that Fe₂O₃ is the most active catalyst in soot oxidation. However, all the catalysts examined are active in transformation of carbonizate components. It has been shown that DTA and TG methods can be used as fast methods testing the carbonizate oxidation. This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal behaviour and vibrational characterization of MH2(IO3)3 phases (M=K,Rb and NH4)

The thermal behaviour of the MH₂(IO₃)₃ (M=K, Rb and NH₄) isomorphous compounds, as well as the IR and Raman spectra have been investigated as part of a study of the properties of solid protonic conductors. Detailed stoichiometries, sustained by TG, DTA, XRD and IR analysis, have been developed into the three phases. There were also evidences of the formation of the [I₃O₈]^– polymeric phases. Their stabilities were associated to the different polarizing power of the H, K and Rb cations.This work was supported by CONICET (Programa QUINOR) and CICPBA.     

Syntheses and reactions of the bis-boryloxide O(Bpin)2(pin = O2C2Me4)

The reaction of the phosphine oxides, OPEt31 and OPn-Bu32 with pinacolborane (HBpin) results in phosphine oxide reduction and the formation of O(Bpin)23. In contrast, the phosphine oxide OPn-Bu3 reacts with HB(C6F5)2 or B(C6F5)3 to give only the donor-acceptor adducts. Compound 3 reacts with HNPt-Bu3 to give the phosphinimonium borate salt, [t-Bu3PNH2][(Bpin(OBpin)2]6, while reaction with Cp2ZrMe2 affords the species Cp2Zr(OBpin)27.