[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.     

二维层状金属碲化物[Mn(en)3]Ag6Sn2Te8的制备及其晶体结构的分析

鉴于硫族金属化合物特殊的物理化学性质及其在半导体材料、催化剂研究、高温超导材料等高科技领域的诸多应用,在近十年内,人们竞相研究,合成出了成百上千新的二元、三元、四元的金属硫化物,金属硒化物和金属碲化物.高温直接反应方法是制备金属碲化物的一种最常用的方法,如:K2BaSnTe4,RbTaCu2Te4,K2Ag2SnTe4,K2HgSnTe4等均是在400～500℃左右的温度下,以单质元素与二元的碲化物直接反应得到的.在该领域中,近年来低温合成技术,如电解法[1],水热法[2]的应用日益受到重视.采用以有机物为溶剂的低温合成技术是90年代以来才取得发展并逐渐成熟起来的.如RbHgSbTe3[3],Rb2Hg3Te4[4]都是采用该低温合成技术而制备成功的.有机溶剂热生长技术与传统的水热法(Hydrothermal)不同之处在于可以根据实验的需要而选用具有不同沸点、带有不同极性及不同官能团的有机溶剂,从而拓宽了该技术的应用范围.本文报道的[Mn(en)3]Ag6Sn2Te8就是以乙二胺为溶剂,以SnTe,MnCl2,AgCl与Te为原料,在180℃下反应得到的.     

一维链状氧族化合物［Mn(en)3］CdSnTe4的制备及其半导体性质的研究

The solvothermal technique was used for the synthesis of ［Mn(en)₃］CdSnTe₄ (Ⅰ). The crystal structure has been determined by single crystal X-ray diffraction techniques. The crystal belongs to the triclinic, space group P1(No.1     

二维层状金属碲化物[Mn（en）3]Ag2Sn2Te8的制备及其晶体结构的分析

鉴于硫族金属化合物特殊的物理化学性质及其在半导体材料、催化剂研究、高温超导材料等高科技领域的诸多应用,在近十年内,人们竞相研究,合成出了成百上千新的二元、三元、四元的金属硫化物,金属硒化物和金属碲化物.高温直接反应方法是制备金属碲化物的一种最常用的方法,如:K2BaSnTe4,RbTaCu2Te4,K2Ag2SnTe4,K2HgSnTe4等均是在400～500℃左右的温度下,以单质元素与二元的碲化物直接反应得到的.在该领域中,近年来低温合成技术,如电解法[1],水热法[2]的应用日益受到重视.采用以有机物为溶剂的低温合成技术是90年代以来才取得发展并逐渐成熟起来的.如RbHgSbTe3[3],Rb2Hg3Te4[4]都是采用该低温合成技术而制备成功的.有机溶剂热生长技术与传统的水热法(Hydrothermal)不同之处在于可以根据实验的需要而选用具有不同沸点、带有不同极性及不同官能团的有机溶剂,从而拓宽了该技术的应用范围.本文报道的[Mn(en)3]Ag6Sn2Te8就是以乙二胺为溶剂,以SnTe,MnCl2,AgCl与Te为原料,在180℃下反应得到的.     

以有机溶剂热生长技术制备金属硫族化合物[Mn(en)_3]PdSe_2及其晶体结构分析

以有机溶剂热生长技术 (solvothermaltechnique) ,即在 180℃乙二胺 (en)溶液中 ,以MnCl3,PdCl2 ,K2 Se在密闭容器中反应 7d ,制备出新的硫族化合物 [Mn(en) 3]PdSe2 ,其阴离子基团为 [PdSe2 ]2 -,阳离子基团为过渡金属Mn与乙二胺 (en)的配合物 :[Mn(en) 3]2 +.以单晶X射线衍射技术解得该晶体结构属正交晶系 ,空间群为Pbcn ,[Mn(en) 3]·PdSe2 (Ⅰ )的晶胞数据 :a =1.1484( 2 ) ,b=1.5 0 5 7( 3 ) ,c =0 .93 62 2 ( 19)nm ,Z =4.     

金属硫族化合物CsSb2(Se2)0.5Se3的溶剂热合成及其晶体结构分析

以有机溶剂热生长技术(Solvothermal Technique)在180 ℃乙二胺(en)溶液中以SbCl₃与碱金属硒化物Cs₂Se和Se在密闭容器中反应7 d,制备出新的金属硫族化合物CsSb₂(Se₂)_0.5Se₃。以单晶X射线衍射技术测得晶体结构属三斜晶系,空间群为P1,晶胞参数：a=0.653 0(2) nm,b=0.707 1(3) nm,c=0.979 9(4) nm,α=80.37(3)°,β=86.28(3)°,γ=74.61(3)°,V=0.430 0(3) nm³,Z=2。     

有机杂化锑硒化合物的溶剂热合成与晶体结构

自1996年Kanatzid is以有机胺为结构导向剂,第一次用溶剂热法合成了含过渡金属钴的锑硫化物[Co(en)3]CoSb4S8[3]以来,水热和溶剂热技术逐渐成为合成多元金属硫属化物的重要方法[1-7]。本文以FeC l2·4H2O、Sb和Se为原料,在乙二胺中于140℃进行溶剂热反应,合成了锑硒化合物[Fe(e     

镉汞四元硒化物K8Cd2.79Hg9.21Se16和Rb4Hg3.04Cd2.96Se8的溶剂热合成及表征

利用溶剂热法合成了2种含镉汞的二维(2D)四元硒化物K8Cd2.79Hg9.21Se16(1)和Rb4Hg3.04Cd2.96Se8 (2)。单晶X射线衍射分析表明,化合物1为正交晶系,空间群为Pbcn,a=1.082 71(17) nm,b=0.678 73(10) nm,c=1.415 0(2) nm,Z=1;化合物2为正交晶系,空间群为Ibam,a=0.640 72(10) nm,b=1.160 25(16) nm,c=1.452 0(2) nm,Z=2。化合物1中含有八元环Cd2Hg2Se4和六元环CdHg2Se3阴离子层(Cd2.79Hg9.21Se16)n8n-;化合物2中含有八元环Cd2(Cd/Hg)2Se4及四元环CdHgSe2和(Cd/Hg)2Se2阴离子层(Hg3.04Cd2.96Se8)n4n-。对这2种化合物进行了扫描电镜和能谱分析、粉末X射线衍射、差示扫描量热分析、固体-可见漫反射光谱和荧光性质等表征。     

有机杂化含Te2^2-／Se3^2-过渡金属化合物的溶剂热合成及晶体结构

本文通过溶剂热法合成了2种新的有机杂化锌碲化物[Zn(dien)2](Te2)(1)和镍硒化物[Ni(dien)2](Se3)(2)(dien=二乙烯三胺),单晶X射线衍射分析结果表明,化合物1属于正交晶系,Cmca空间群,晶胞参数:a=9.212(2),b=10.854(3),c=15.723(4),Z=4。化合物2属于正交晶系,Pna21空间群,晶胞参数:a=18.047(4),b=9.8236(19),c=9.0079(19),Z=4。在两种化合物中,1的阳离子中Zn2 与2个dien螯合形成稍变形的八面体几何构型,阴离子为哑铃型的Te22-。2的阳离子中Ni2 离子与2个dien螯合形成稍变形的八面体几何构型,阴离子为‘V’字型的Se32-。     

碱金属硒化物MHgSbSe~3(M=K,Rb, Cs)的晶体结构及其半导体性 质的研究

用有机溶剂热生长技术(SolvothermalTechnique)制备碱金属硒化物MHgSbSe~3(M=K,Rb,Cs),用单晶X射线衍射技术对其进行晶体结构分析,热分析结果表明,在常温(<200℃)下均为稳定的化合物。光学性质测试表明它们是半导体材料,KHgSbSe~3,RbHgSbSe~3,CsHgSbSe~3的禁带宽度依次为1.85eV,1.75eV,1.65eV。     

Solvothermal Synthesis of Two Cationic Indium Selenides with I− Ion as Counterion

Two new indium selenides [In(en)₂Se]₂·2I ( 1 ) and [In(teta)Se]₂·2I ( 2 ) (en = ethylenediamine, teta = triethylenetetramine) were obtained under mild solvothermal conditions and structurally characterized. Compounds 1 and 2 consist of unusual organic hybrid indium selenide cations and I^? anions. These ions are assembled to two different supramolecular structures by N‐H···I and N‐H···Se H‐bonds, namely extended 3‐D network structure for 1 and extended sheet structure for 2 . The optical band gaps of 2.92 eV for 1 and 3.15 eV for 2 were derived from optical absorption spectra. The thermal stability of 1 and 2 was investigated by thermogravimetric measurements.     

Hydrothermal synthesis of [C6H16N2][In2Se3(Se2)]: A new one-dimensional indium selenide

A new organically templated indium selenide, [C₆H₁₆N₂][In₂Se₃(Se₂)], has been prepared hydrothermally from the reaction of indium, selenium and trans-1,4-diaminocyclohexane in water at 170 °C. This material was characterised by single-crystal and powder X-ray diffraction, thermogravimetric analysis, UV-vis diffuse reflectance spectroscopy, FT-IR and elemental analysis. The compound crystallises in the monoclinic space group C2/c (a=12.0221(16) Å, b=11.2498(15) Å, c=12.8470(17) Å, β=110.514(6)°). The crystal structure of [C₆H₁₆N₂][In₂Se₃(Se₂)] contains anionic chains of stoichiometry [In₂Se₃(Se₂)]²⁻, which are aligned parallel to the [1 0 1] direction, and separated by diprotonated trans-1,4-diaminocyclohexane cations. The [In₂Se₃(Se₂)]²⁻ chains, which consist of alternating four-membered [In₂Se₂] and five-membered [In₂Se₃] rings, contain perselenide (Se₂)²⁻ units. UV-vis diffuse reflectance spectroscopy indicates that [C₆H₁₆N₂][In₂Se₃(Se₂)] has a band gap of 2.23(1) eV.     

链状[NH3CH2CH2NH3]AgAsS4的溶剂热合成及表征

利用溶剂热方法合成了链状[NH3CH2CH2NH3]AgAsS4,通过单晶X射线衍射技术对其进行了晶体结构分析,该化合物晶体属单斜晶系,空间群C2/c,晶胞参数a=1.35805(8)nm,b=0.65331(3)nm,c=2.27711(9)nm,β=106.42(3)°,Z=8.化合物具有有趣的梯子状双链结构,该阴离子链由AsS4与AgS3共用顶点交替连接而成,有机阳离子在阴离子链之间存在较强的N—H…S氢键.DSC和Tg分析结果表明化合物在200℃以下是稳定的.     

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.     

一维链状硫酸铟的溶剂热合成与表征

在溶剂热条件下, 以三乙烯四胺(TETA)作为模板剂, 合成出具有一维链状结构的硫酸铟化合物(C6H22N4)0.5[In(OH)](SO4)2(1). 采用红外光谱、热重分析、ICP、元素分析、粉末X射线衍射及单晶X射线衍射等手段对其进行了表征. 结果表明, 化合物1属于单斜晶系, P2(1)/c空间群, a=1.05240(3) nm, b=1.36802(4) nm, c=0.75295(2) nm, β=101.558(2)°, V=1.06204(5) nm3, Z=4, R1=0.0368, wR2=0.0897, GOF=1.068. 其结构是由InO4(OH)2八面体和SO4四面体通过共顶点连接形成的一维阴离子Tancoite-type 链. 质子化的TETA阳离子通过与阴离子链中的O原子之间的氢键作用将一维链连接成为三维超分子结构.     

Solvothermal Synthesis,Crystal Structure and Properties of a New Organic Templated Lanthanum Sulfate [C4N3H16][La(SO4)3(H2O)]

A new organic templated lanthanum sulfate [C₄N₃H₁₆][La(SO₄)₃(H₂O)] ( 1 ) has been solvothermally synthesized by using n‐butanol as solvent. The colorless block crystals were characterized by IR, TGA, ICP, and XRD. The structure was determined by single‐crystal X‐ray diffraction: Monoclinic, P2₁/c, a = 10.8878(19), b = 15.478(3), c = 9.9639(18) Å, β = 114.062(2)°, V=1533.2(5) ų, Z = 4]. Crystal structure analysis shows that the one dimensional chain of 1 consists of the LaO₉ polyhedra and the sulfate groups. Coordination water molecules link adjacent chains by using hydrogen bonds to generate 2D layers, whereas the organic amines are inserted between the layers. The formation of 1 demonstrates that solvents play an important role during the synthesis.     

Solvothermal Synthesis and Crystal Structure of Mn2(C5H14N2)Sb2S5: A New Member of the Mn2(L)Sb2S5 Family (L is an Organic Structure Director)

The new compound Mn₂(C₅H₁₄N₂)Sb₂S₅ (C₅H₁₄N₂ = 1,3‐diaminopentane, DAPE) was prepared under solvothermal conditions using the elements as starting materials. The compound crystallizes in the orthorhombic space group Pbca with the lattice parameters a = 12.620(3), b = 11.877(2) and c = 21.814(4) Å. The primary building units are trigonal SbS₃ pyramids and distorted MnS₆ and MnS₄N₂ octahedra. These primary building blocks are joined to form Mn₂Sb₂S₄ hetero‐cubane units which are then connected via common corners, edges and faces thus forming a second type of hetero‐cubane. The hetero‐cubanes are condensed into layers within the (001) plane. The connection mode yields ellipsoidal pores within the layers with dimensions of about 9·7.5Å. The N atoms of the structure directing amines are exclusively bound to one of the two crystallographically independent Mn²⁺ cations and they point into the pores and between the layers separating the layers from each other. The interlayer separation measures about 6.7Å. Whereas the MnS₆ octahedron shows only a moderate distortion the MnS₄N₂ octahedron is severely distorted with a remarkable long Mn‐S bond length of 2.968Å.     

Solvothermal Synthesis and Characterization of （ NH3 CH2 CH2 NH3） HgSnS4 with a Column Structure

IntroductionSulfide-based open-framework materials are in-triguing compounds.They possess very diverse and in-teresting structures,and exhibit potential applicationsas a newgeneration of molecular sieves with the proper-ties of semiconductor materials[1].…     

[VO(dien)]2GeS4: Solvothermal Synthesis and Crystal Structure with an Ortho‐Thiogermanate as Tetradentate Ligand

The compound [VO(dien)]₂GeS₄ ( 1 , dien = diethylenetriamine) features an ortho‐thiogermanate anion [GeS₄]^4–, which acts as tetradentate ligand joining [VO(dien)]^2– complexes. The compound was obtained under solvothermal conditions crystallizing in thenon‐centrosymmetric orthorhombic space group Pna2₁ with a =19.8310(11), b = 8.0814(5), c = 12.0889(9) Å, V = 1937.4(2) ų and Z = 4. The V⁴⁺ cations are in a distorted octahedral environment of a tridentate dien molecule, one oxygen atom and two sulfur atoms from the [GeS₄]^4– anion. A three‐dimensional network is generated by hydrogen bonding interactions.