Solvothermal Synthesis,Characterzation And Crystal Structure Of Multinary Stannum Chalcogenides

Most Metal chalcogenide compounds because of its thermodynamically metastable structures,have complex structure and special properties.These compounds have good application prospects in the field of semiconductor,light emission,photoluminescence,nonlinear optics,optoelectronics,molecular sieve,ion exchange,chemical adsorption.In recent years,becoming one of the increasingly studied inorganic multifunctional materials.And therefore the synthesis of these compounds has become research hot topics in the study of inorganic chemistry.Solvothermal（hydrothermal）synthesis method is an effective method to obtain the metastable structures.Many new structure and special nature metal chalcogenide compounds can be obtained by utilizing this method.（1）In ethylenediamine solvent system,under 180℃temperature condition,synthesized two kinds of compound of[Co（en）₃]₂Sn₂Se₄S₂（1）and[Mn（en）₃]₂Sn₂Se₄S₂（2）.Single crystal X-ray diffraction results show that compounds 1 and 2 have similar crystal structure both orthorhombic,belongs to Pbca space group,and both containing dimer anion,which contains S,Se two kinds of chalcogen elements.The crystal lattice parameters were as follows:compound 1,a=1.5491（5）nm,b=1.8666（6）nm,c=1.1842（6）nm,Z=8;compound 2,a=1.1688（4）nm,b=1.6020（8）nm,c=1.9658（10）nm,Z=8.（2）Use 2,3-dimercaprol dimercaptopropanol as chelating agent,in1,4-diaminobutane and pyridine solvent system,under 180℃condition,obtain the metal chelcogenide of Cs₈Sb₆Sn₄S₄Se₁₇（3）.Single crystal X-ray diffraction results indicated that compound Cs₈Sb₆Sn₄S₄Se₁₇（3）was monoclinic,belongs to C2/c space group,and composed of cationic Cs⁺and infinite chain anionic(Sb₆Sn₄S₄Se₁₇)^8-.The crystal lattice parameters were as follows:a=2.6127（16）nm,b=0.9073（6）nm,c=1.9062（12）nm,β=91.425°,Z=4Three kinds of compounds’powder X-ray diffraction analysis showed that all of them were pure phases;The results of thermal analysis showed that three kinds of compounds have better thermal stability;UV-Vis diffuse reflectance spectra showed that three compounds have semiconductor properties.And respectively discussed influence factors of the synthesis,and summed up the optimum synthesis conditions.（3）Based on the above synthetic routes,use 1,2-ethanedithiol as chelating agent,in 1,4-diaminobutane system,under 190℃condition,obtain the indium-antimony chalcogenide of InSbSe₂S（4）.The compounds were analyzed by scanning electron microscope and energy dispersive spectrum analysis and single crystal X-ray diffraction analysis.Single crystal X-ray diffraction results indicated that compound InSbSe₂S（4）was monoclinic,belongs to Cm space group,and containing interesting two-dimensional layer structure.The crystal lattice parameters were as follows:a=3.004（6）nm,b=0.3909（3）nm,c=0.8842（4）nm,β=91.425°,Z=4.