溶剂热合成磷酸亚铁锂的研究

以溶剂热方法首次合成了橄榄石相的磷酸亚铁锂,并以水热法为参照.使用XRD,TEM和FT-IR等手段进行表征.溶剂热法制备的样品呈球形或多面体状.而水热法制备的颗粒则由纤维状成长为菱形.两种方法产物的形状差异可能是由于溶剂热反应体系中较高的压力抑制了纤维态晶体的产生.溶剂热法和灼烧都有利于磷酸亚铁锂晶相发育.     

微乳辅助的溶剂热法合成磷酸钐纳米棒

自1991年碳纳米管被发现以来,一维纳米材料以其独特的电、磁、光学和机械性质以及在纳米器件和功能材料上的巨大应用潜力而引起全世界的广泛关注,人们通过模板法、溶胶-凝胶法、水热法及微乳液法等多种方法合成了一系列一维纳米材料,其中微乳液法是近几年来兴起的较有发展前景的纳米材料的合成方法,微乳液是由油相、水相、表面活性剂和助表面活性剂组成的均匀稳定的体系,水相在表面活性剂和助表面活性剂的作用下均匀地分散在油相中,     

CdS和CdSe新型纳米结构的高效溶剂热合成

采用快速高效的溶剂热法合成了海星形CdS纳米结构和一维CdSe纳米结构。用XRD、SEM和UV-Vis等表征手段对产物进行了表征，结果表明产物为单一的CdS和CdSe纳米结构，且CdS纳米结构具有良好的分散性，其形成极大地受到pH值影响，而CdSe先形成层状的二维结构、再形成一维纳米结构。     

溶剂热法合成碳纳米材料

本文综述了溶剂热法合成多种碳纳米管、纳米电缆、纳米棒、纳米球和纳米空心锥的研究现状。350 ℃下用金属钾还原六氯代苯,在用不同催化剂时,可分别得到碳纳米管和碳球,碳球的形成可以解释为石墨层的微条卷曲而成。600 ℃下金属镁还原乙醇得到了竹节状和Y-型碳纳米管。500 ℃下还原四氯化碳和碳酸钠可得到平均直径为100 nm的碳纳米管。700 ℃下金属锌还原乙醚制成了左右螺旋型交织的碳纳米管。在硫的存在下,200 ℃以下二茂铁热解成非晶碳纳米管和Fe/非晶碳纳米同轴电缆。     

溶剂热法合成硫化铜花状微米球超结构及其光催化性能

以氯化铜(CuCl₂•2H₂O)和硫脲(CH₄N₂S, Tu)为原料, 乙二醇(C₂H₆O₂)为溶剂, 用溶剂热法于140 ℃反应90 min成功制备了直径为2.2～4.8 µm由纳米片组成的花状硫化铜(CuS)微米球超结构. 用XRD, SEM, TEM, SAED, HRTEM以及UV-Vis等手段对产品进行了表征|以氙灯和高压汞灯为光源, 亚甲基蓝为目标降解物评价了CuS超结构的光催化活性. 结果表明, 所制备的产品是六角相的CuS, 经计算, 其晶胞参数为a＝0.3813 nm, c＝1.6774 nm|所用溶剂、硫源、铜源及反应温度、反应时间对产品的形貌均有较大影响|UV-Vis分析表明, CuS微米球超结构的带隙能量为2.0 eV|光催化性能测试表明, 所制备的CuS微米球超结构在紫外光区和可见光区均具有较高的光催化活性, 但在可见光区的光催化活性更高, 在35 W氙灯和450 W的高压汞灯下, 光照30 min, 亚甲基蓝的降解率分别达到98.7%和82.9%. 此外, 还讨论了硫化铜微米球超结构可能的形成机理.     

溶剂热/水热条件下空旷结构草酸锌的合成

应用水热法及溶剂热方法，选择两种模板剂1，2-丙二胺和4，5-二氮芴-9-酮连氮(L)设计合成了草酸锌空旷结构材料[Zn₂(C₂O₄)3][C₃H₁₂N₂]·H₂O (Ⅰ)和[Zn₂(C₂O₄)₃]·L·6[H₃O] (Ⅱ)，使用CHN元素分析、     

溶剂热法合成ZnSe纳米球

以乙酸锌和Se粉为原料,环己酮为溶剂,于180 ℃反应24 h制得黄色纳米球ZnSe,其结构和性能经XRD,SEM及TEM表征.     

溶剂热法合成花朵状钴磁性粉体及表征

采用一种简单的溶剂热法成功的合成了花朵状的钴磁性粉体。通过X射线粉末衍射(XRD),扫描电子显微镜(SEM)等对样品进行物相与形貌的表征。结果表明样品为六排堆积(hcp)和面心立方结构(fcc)混合结构的钴单质,形貌为由很多个厚度约为50～150 nm的菱形花瓣构成的花朵状结构,每个花朵的尺寸约为2μm左右。采用振动样品磁强计(VSM)测试了样品的磁性能,测试表明样品在室温下表现出铁磁性,饱和磁化强度(Ms)为140 emu.g-1,剩磁(Mr)为9.4 emu.g-1,矫顽力(Hc)为280 Oe。     

溶剂热法合成花状分级结构LiFePO_4及其电化学性能研究

以乙二醇/水为溶剂,酒石酸铵为添加剂和碳源,采用溶剂热法,制备了高振实密度(1.3 g·cm-3)的锂离子正极材料磷酸铁锂(LiFePO4)。采用X射线衍射(XRD)、红外光谱、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对样品进行了表征。研究结果表明样品为单晶纳米片组装而成的花状三维多孔分级结构LiFePO4。通过时间单因素实验探讨花状分级结构LiFePO4的生长机理,其生长过程概括为:成核和生长,定向组装。电化学性能测试结果表明LiFePO4样品具有优异的倍率性能(10C时放电比容量保持在74.8 m Ah·g-1)与循环性能(50次循环后容量保持率93%)。     

Solvothermal Synthesis,Crystal Structure,and Properties of a New Organic‐Templated Holmium Sulfate with 1D Single Ladder Chains

A new organic amine templated 1D holmium sulfate (C₂H₈N)[Ho(SO₄)₂ · H₂O] ( 1 ) has been synthesized and solvothermally and structurally characterized by single‐crystal X‐ray diffraction, IR spectroscopy, thermogravimetric and X‐ray diffraction analyses as well as scanning electron microscopy (SEM). The structure of framework 1 is constructed from HoO₈ polyhedra and SO₄ tetrahedra. S(1) and S(2) connects Ho(1) and its crystallographic partners by using three S–O–Ho linkages to generate double chains, whereas the adjacent double chain are connected by μ₃‐O (O₅) atoms to form a novel single ladder chains.     

Solvothermal Synthesis of a New Amine-Templated Vanadium Sulfate

A new organic-templated vanadium sulfate with formula [C₄H₁₂N₂][V^III (OH)(SO₄)₂] · H₂O 1 has been prepared under solvothermal conditions by using a mixture of glycol and water as solvent. The structure of this compound was characterized by IR, element analysis, TG and single crystal X-ray diffraction. The title compound crystallizes in the space group monoclinic, P2₁/c, a = 9.290(4) Å, b = 18.264(7) Å, c = 7.132(3) Å, β = 98.149(8)°,V = 1197.88 Å³, Z = 4. Structural analysis indicates that the title compound 1 possesses a 1D chain structure formed by VO₆ octahedra and SO₄ tetrahedra.     

A New Organo-Directed Titanium Phosphate Phase Containing Zigzag Chains of Corner-Sharing TiO_6 Octahedra

The chemistry of titanium phosphates has attracted considerable interests because of their applications in ion exchange, redox catalysis and outstanding non-linear optical materials. However, only a few titanium compounds have been reported, and fewer reports deal with single-crystal structure determinations due to the difficulty in obtaining large single crystals of titanium phosphates. The synthesis of titanium phosphates often leads to two-dimensional layered phases1-3, and several titanium…     

具有开放骨架结构氟化磷酸钛的水热合成及分子动力学辅助确定骨架中模板剂的位置

在水热体系中,制备了一个具有三维开放骨架结构的氟化磷酸钛化合物Ti₄(PO₄)4(HPO₄)₂F₂.[(CH₃)₂N(CH₂)₂NH₃][H₃O](简称TP-J3J=Jilinuniversity).用X射线粉末衍射、元素分析、热重分析和X射线单晶衍射对其进行了表征.单晶结构分析表明,该化合物属于三斜晶系,P1空间群,晶胞参数a=0.6353(1)nm,b=0.8699(2)nm,c=1.1069(2)nm,α=93.94(3),β=90.13(3),γ=107.96(3),V=0.5804(2)nm³,Z=2,R₁=0.0391,wR₂=0.0959,GOF=1.052.TP-J3的骨架结构可以看作是由次级结构单元(SBU)[Ti₂(PO₄)₂(HPO₄)F]通过氧桥共顶点相连构筑而成的,在a和c方向形成了两种不同的八元环孔道,两种孔道相互交叉,形成了一种“类笼”结构.通过计算模拟确定双质子化的模板剂存在于“类笼”中,模板剂与骨架原子之间存在强烈的氢键作用,可稳定骨架的结构.     

Solvothermal Synthesis and Crystal Structure of Zn（en）3 B5O7（OH）3

Introduction Boratecompounds,inwhichboronisboundonly tooxygen,areofconsiderablemineralogicalandindus trialimportance.Thesecompoundscontaininganionic componentscomposedofBO3andBO4groups,which maybelinkedtogetherbysharingoxygenatoms,can formisolatedringsand…     

Solvothermal Syntheses and Structure of a New Polyoxomolybdate Functionalized with Carboxyphosphonate

A new functionalized polyoxomolybdate [(HOOCC₅H₉NCH₂PO₃)₂Mo₅O₁₅]^4– ( 1 ) was synthesized by solvothermal reaction at 120 °C and structurally characterized by X‐ray single‐crystal diffraction, X‐ray powder diffraction as well as with infrared spectroscopy, elemental analysis, and thermogravimetric analysis. The title polyoxoanion consists of a ring of five distorted MoO₆ octahedra linked through four edge‐sharing and one corner‐sharing junctions. Two pending carboxyphosphonate ligands are attached on opposite sides of the ring by the two PO₃ groups. As a result the two dangling arms with their terminal carboxylate groups protrude away from the {Mo₅O₁₅} framework in diametrically opposed directions. Each Mo₅‐ring is further connected to adjacent Mo₅‐ring through hydrogen bonds, which consist in the protonated nitrogen atoms, the carboxyl oxygen atoms from L^3– ligands and oxygen atoms from {Mo₅O₁₅} cluster to form a 2D framework structure.     

Solvothermal Synthesis,Crystal Structure and Properties of the First Organic‐templated Holmium Sulfate [C2N2H10]3[Ho2(SO4)6·2H2O]

The first organic amine‐templated holmium sulfate [C₂N₂H₁₀]₃[Ho₂(SO₄)₆·2H₂O] ( 1 ) has been synthesized solvothermally and has been structurally characterized by single‐crystal X‐ray diffraction studies, IR spectroscopic, thermogravimetric (TG) and inductivity coupled plasma (ICP) measurements. Crystal analyses of compound 1 showed a novel inorganic layer constructed from the zigzag and helical [–Ho–O–S–O–]_n chains, both of the chains are connected by μ‐2 SO₄^2– groups to form 10‐membered rings. The solvent plays an important role during the formation of 1 .     

Hydrothermal Synthesis and Crystal Structure of a New Sandwich—type Molybdenum Phosphate

1 INTRODUCTION The synthesis of porous and open-framework transition metal phosphates has received great in- terest due to their various compositions and topolo- gyies, as well as their useful properties such as con- trollable size- and shape-selectivity, rigid frame- works and chemical/thermal stability[1]. Of these phosphates constructed from oxometal polyhedra and PO4 tetrahedron, the most interesting is the [MoV6P4X31]n－ (X=O, OH) family with the dimen- sionalities ranging from …     

NaVPO5晶体的水热合成与结构研究

通过在水热合成体系中加入还原剂,利用五价钒化合物成功地合成出纯相NaVPO₅晶体,并用电子顺磁共振和四圆衍射对其进行了表征.     

非水体系中磷酸钴大单晶的合成与结构

非水体系中磷酸钴大单晶的合成与结构徐家宁，袁宏明，卜卫名，邵一鸣，宋天佑，樊玉国，徐如人（吉林大学化学系超分子结构与谱学开放实验室，长春，１３００２３）关键词磷酸钴，大单晶，非水体系，晶体结构近年来的研究结果表明，非水合成技术对合成具有开放骨架结构的...