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利用水热技术合成了2个新型钴支撑的磷钼多金属氧酸盐超分子化合物:(C2N2H10)5[(P4Mo6O25(OH)6)2Co](1)和(Co(H2O)6)2(C5NH6)6[(P4Mo6O25(OH)6)2Co]·10H2O(2).并通过元素分析、红外光谱、热重分析和X射线单晶衍射对2个化合物进行了表征.结果表明:化合物1属于三斜晶系,P-1空间群;晶胞参数a=1.179 9(2)nm,b=1.337 7(2)nm,c=1.479 7(3)nm,α=73.435(2)°,β=74.383(2)°,γ=66.499(2)°,V=2.020 5(6)nm3,F(000)=1 327,Z=1;化合物2属于属于三斜晶系,P-1空间群;晶胞参数a=1.220 68(11)nm,b=1.381 08(13)nm,c=1.687 18(15)nm,α=92.275(1)°,β=104.774(1)°,γ=114.475(1)°,V=2.468 8(4)nm3,F(000)=1 649,Z=1. 相似文献
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介绍了近几年来多金属氧酸盐(polyoxometalate,缩写为POM)在合成化学研究方面的新进展,内容包括:由水热合成方法得到的Keggin型[SiNb12O40]16-及其与[Ti2O2]4 连接构成的一维链状结构及[H2Si4Nb16O56]14-簇;Silverton型多阴离子[GdMo12O40]9-及三维网络结构;POM和过渡金属簇通过有机π共轭体系形成的杂化材料;一步法自组装合成的四核轮状的多金属钨酸盐;控制合成得到具有蛋白质尺寸的Mo368氧簇和开普勒环形山结构的多钼氧簇;用{P2W12}杂多阴离子作为建筑块合成出的含有20个Cu中心的大轮型POM;用常规方法突破“氧墙”效应,获得的第一例稳定的含有第三过渡金属元素的多金属氧酸盐;通过逐步合成法用[SiW9O34]10-作为建筑单元合成出二聚和四聚的POM化合物;合成带有均匀孔道结构,具有选择性吸附和分离混合低碳脂肪醇和低碳氰分子的三维网络结构等. 相似文献
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A new kind of Anderson-type chromium-molybdates containing the rare earth elements are synthesized, which have the general molecular formula of (NH4)6[CrMo5Ln(OH2)2O24H6]·xH2O (Ln=La,Ce,Pr,Nd,Sm,Gd and Yb). The components of these heteropoly complexes are determined by chemical elemental analysis, ICP and TG-DTA. And IR, UV, ESR,XPS and 1H NMR are also applied to characterize the complexes as well. The results indicate that the structures of these complexes are Anderson B type and the rare earth elements are in the inner sphere of the heteropoly salts. The thermal stabilities of these complexes studied by TG-DTA show that the range of pyrolysis temperature is between 490℃ and 500℃. 相似文献
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在水热条件下合成了一种新型无机-有机杂化物{[Cu(phen)2][Cu(phen)(H2O)]2P2Mo5O23}.6H2O,通过元素分析、红外光谱、热重分析和X射线单晶衍射方法确定了其晶体结构.结构分析表明:该晶体属于三斜晶系,P1-空间群,晶胞参数a=1.224 54(12)nm,b=1.435 86(14)nm,c=2.009 3(2)nm,α=80.192(2)°,β=74.585(2)°,γ=67.025(2)°,V=3.126 7(5)nm3,Z=2. 相似文献
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A novel hexa-NiⅡ substituted trilacunary Keggin polyoxometalate [{Ni6(μ3- OH)3(en)3(H2O)6}(B-α-PW9O34)]-6H2O 1 (en = ethylenediamine) has been hydrothermally synthesized and characterized by IR spectra, elemental analysis, thermogravimetric analysis (TGA), single-crystal X-ray diffraction and magnetic property. Compound 1 crystallizes in the hexagonal space R3c with a = 20.4124(5), c = 21.4427(4)A, γ = 120.000°, V = 7737.5(3)A3, Z = 6, GOF = 1.083, R (wR) = 0.0317 (0.0610). Single-crystal X-ray diffraction indicates that 1 contains a hexa-Nin substituted trivacant Keggin [{Ni6(μ3-OH)3(en)3(H2O)6}(B-α-PW9O34)] unit. The magnetic study shows the presence of ferromagnetic coupling interactions within hexa-Nin clusters with J1 = 0.69 cm-1 and J2 = 0.92 cm^-1 for 1. 相似文献
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Two new hybrid polyoxotungstates, [Co(2,2'-bipy)3][a-H5PW11CoO40]-3H2O 1 and [Fe(2,2'-bipy)3]2[a-HBW12O40]-2.5H2O 2 (2,2'-bipy = 2,2'-dipyridyl), have been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray structural analyses. The results of X-ray crystallography analyses exhibit that 1 consists of one a-Keggin anion [a-H5PW11CoO40]2- and one isolated [Co(2,2'-bipy)3]2+ complex, while 2 is constructed from one a-Keggin anion [a- HBW12O40]4- and two isolated [Fe(2,2'-bipy)3]2+ cations. The data for 1: orthorhombic system, space group Pbcn, a = 16.062(6), b = 27.278(10), c = 16.951(6)A, V = 7427(5)A3 and Z = 4; and those for 2: triclinic system, space group P1, a = 13.787(3), b = 17.857(5), c = 18.918(5)A, a = 88.009(12), β = 72.768(10), γ = 74.935(10)°, V = 4291(2)A3 and Z = 2. 相似文献
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A 4, 4'-bipyridine bridging dumbbell-like dimeric pentamolybdate [4, 4'-H2bipy]3[4,4'-Hbipy]2[(Mo5O17)2(4,4'-bipy)] has been synthesized by hydrothermal synthesis and characterized by elemental analysis, IR spectrum, UV spectrum, TG and X-ray crystallography. The title compound crystallizes in triclinic, space group P(-1) with a = 10.578(2), b = 11.047(2), c = 16.576(3) (A), α = 79.86(3), β = 75.34(3), γ = 79.40(3)°, C60H58Mo1oN12O34, Mr = 2450.58, V = 1824.8(6) (A)3, Z = 1, Dc = 2.230 g/cm3, F(000) = 1194, μ = 1.757 mm-1, the final R = 0.0252 and wR = 0.0559 for 5506 observed reflections with I > 2σ(Ⅰ). The structural analysis indicates that the title compound contains a novel polyanion [(Mo5O17)2(4,4'-bipy)]8-, in which two identical (Mo5O17)4- anions are buttressed by a 4,4'-bipyridine molecule through Mo-N bond. 相似文献
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1 INTRODUCTION Polyoxometalates (POMs) have been attracting extensive interest of many chemists in solid-state materials chemistry owning to the various structures and great potential applications in catalysis, medi- cine, photo-electricity and magnetism[1~9]. Over the past decades, lots of novel POMs have been pre- pared by hydrothermal synthesis, such as discrete structure[10], one-dimensional chain-like structure[11, 12] and higher dimensional architecture[13~18]. However, in these… 相似文献
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用水热方法合成了新型的硅钨杂多氧酸盐(C2H10N2)3(SiW12O40)·3H2O,用元素分析、IR和单晶X射线衍射分析技术对化合物的分子和晶体结构进行了表征。 结果表明,该化合物的晶体属于三斜晶系,P1空间群,a=1.3193(3) nm,b=1.3198(3) nm,c=1.3193(3) nm,α=76.05(3)°,β=76.13(3)°,γ=76.05(3)°,V=2.1231(7) nm3,Z=1,R1=0.0518,wR2=0.1355。 化合物分子由一个α-Keggin结构的硅钨多金属簇阴离子、3个乙二胺分子作为平衡阳离子和3个结晶水分子组成,簇阴离子的端氧与乙二胺阴离子及结晶水分子之间的多种类型的氢键连接形成三维超分子结构。 化合物磁性测量表明,其分子内存在反铁磁性相互作用。 相似文献
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在水热条件下合成了一种新的二帽二支撑的Keggin型钼钒多金属氧酸盐[Cu(2,2'-bpy)3]{[Cu(2,2'-bpy)2]2HPⅤMo 8 VI V 6 IV O42]}·2H2O(1,bpy=联吡啶),利用元素分析、红外光谱、X射线光电子能谱,粉末和X射线单晶衍射等分析技术对化合物的晶体结构进行了表征。 结果表明,该化合物属于单斜晶系,C2/c空间群,a=2.8734(3) nm,b=1.47333(12) nm,c=2.31023(16) nm,β=112.509(5)°,V=9.0351(12) nm3,Z=1,R1=0.0489,wR2=0.1286。 化合物的阴离子是二帽α-Keggin结构P/Mo/V多金属氧簇,通过簇阴离子两个钒帽上的端氧分别支撑两个铜过渡金属配合物,化合物簇阴离子,水分子和2,2'-联吡啶分子之间通过π-π和氢键作用形成了三维超分子结构。 相似文献
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溶剂热合成法制备(Zn,Hg)S微晶和薄膜 总被引:4,自引:0,他引:4
近年来,由于Ⅱ~Ⅵ族半导体纳米材料的特殊物理、化学性质及其在半导体、光学器件、激光二极管、IR探测器等方面的广泛应用,它们的制备和表征引起了人们越来越大的兴趣犤1~11犦。现在(Zn,Hg)S微晶正被广泛而深入的研究和应用。例如:一种发蓝光的激光二极管已经设计成功,它包含一夹在两衬层间的活性层,无论是在衬层还是在活性层中都包含有(Zn,Hg)S犤5犦。Sugao也曾报道过一种以(Zn,Hg)S为基础的半导体激光器件犤6犦。Parkin曾用MCl2(M=Zn,Cd,Hg)和Li2E(E=O,S,Se,Te)混合热解法制备ME或MxM'yS… 相似文献
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利用Na2MoO4·2H2O,MoO3,乙二胺,和H2O通过水热合成法合成了一维锯齿状化合物[(en)2(Mo6O20H4)]n.晶体解析表明,该化合物属于单斜晶系,P21/n空间群,a=0.80680(16)nm,b=1.4371(3)nm,c=0.88874(18)nm,β=97.89(3)°,V=1.0207(4)nm3,Z=2,Dc=3.305Mg·m-3,μ=3.681mm-1,F(000)=960.该化合物结构单元由二个游离的乙二胺分子和一个阴离子Mo6O4-20阴离子中,六20构成.在Mo6O4-个钼原子和八个相邻的氧原子构成两个八员环,在每个八员环的两侧分别存在着一个与三个钼原子相连的桥氧. 相似文献
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水热条件对板钛矿相二氧化钛微结构的影响 总被引:1,自引:0,他引:1
以四氯化钛和氢氧化钠为原料制备TiO2前驱体,通过水热法合成了不同形貌板钛矿相TiO2,利用X射线衍射和透射电镜对所得样品进行了表征。研究了反应初始pH值、水热反应温度和水热反应时间对TiO2形貌、物相和晶粒尺寸的影响。结果表明,pHinitial是决定TiO2粉体物相、粒径和形貌的主要因素。随着水热反应温度的升高和水热反应时间的延长,板钛矿相TiO2的晶粒逐渐长大。pHinitial的增大,导致无定形TiO2转化成板钛矿相所需的水热温度升高,水热时间变长;同时,所形成板钛矿相TiO2的晶粒尺寸和颗粒粒径也较大。XRD和TEM结果表明,板钛矿相TiO2颗粒是由多个纳米微晶组成的聚集体。当pHinitial为9.00~12.00时,200 ℃下水热反应24 h合成了纯板钛矿相TiO2。 相似文献