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化学学报
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化学学报 ›› 2005, Vol. 63 ›› Issue (19): 1829-1833. 上一篇    下一篇

研究论文

层状MAgTeS3 (M＝K, Rb)的溶剂热合成与表征

白音孟和1，叶玲2，季首华3，安永林*,1，宁桂玲1   

  1. (1大连理工大学化学系 大连 116024)
    (2吉林大学超分子结构与材料教育部重点实验室 长春 130012)
    (3大连理工大学材料系 大连 116024)
  • 投稿日期:2005-01-19 修回日期:2005-06-03 发布日期:2010-12-10
  • 通讯作者: 安永林

Solvothermal Synthesis and Characterization of MAgTeS3 (M＝K, Rb) with Layered Structure

BAIYIN Meng-He1, YE Ling2, JI Shou-Hua3, AN Yong-Lin*,1, NING Gui-Ling1   

  1. (1 Department of Chemistry, Dalian University of Technology, Dalian 116024)
    (2 Key Lab of Supramolecular Structure and Materials of Ministry of Education, Jilin University, Changchun 130012)
    (3 Department of Materials, Dalian Uni-versity of Technology, Dalian 116024)
  • Received:2005-01-19 Revised:2005-06-03 Published:2010-12-10
  • Contact: AN Yong-Lin

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以硫醇为螯合剂, 在溶剂热条件下合成了两种层状硫代亚碲酸盐KAgTeS3 (1)和RbAgTeS3 (2). X射线单晶解析表明, 1和2是类质同晶化合物. 在晶体结构中, 银硫四面体通过共用顶点形成无限的平行链, 在相邻链中银硫四面体取向相反, 这些链与链由三角锥配位的碲互相连接形成阴离子层状结构, 阳离子在阴离子层间. 1的结晶学数据为: Mr＝370.75, P21/c, a＝0.73639(6) nm, b＝1.06468(8) nm, c＝0.85203(6) nm, β＝106.4640(10)°, V＝0.64062(8) nm3, Z＝4, R(F)＝4.44%, wR(F2)＝11.66%. 2的结晶学数据: Mr＝417.12, P21/c, a＝0.75531(12) nm, b＝1.07076(7) nm, c＝0.8583(2) nm, β＝106.497(6)°, V＝0.66558(19) nm3, Z＝4, R(F)＝6.00%, wR(F2)＝15.43%. DSC及紫外-可见漫反射光谱研究表明, 这两种化合物为半导体, 并具有很好的热稳定性.

关键词: 溶剂热合成, 四元金属硫代亚碲酸盐, 晶体结构

Two thio-tellurite KAgTeS3 (1) and RbAgTeS3 (2) were synthesized solvother-mally and characterized by X-ray single crystal diffraction. These isostructural compounds compose of infinite parallel chains formed by AgS4 tetrahedra sharing their vertices, and these chains are further connected by trigonal-pyramidally coordinated Te4＋ to form anionic layered structure with cations located between the layers. Crystal data for 1: Mr＝370.75, P21/c, a＝0.73639(6) nm, b＝1.06468(8) nm, c＝0.85203(6) nm, β＝106.4640(10)°, V＝0.64062(8) nm3, Z＝4, Mo Kα, λ＝0.071073 nm, R(F)＝4.44%, wR(F2)＝11.66%. Crystal data for 2: Mr＝417.12, P21/c, a＝0.75531(12) nm, b＝1.07076(7) nm, c＝0.8583(2) nm, β＝106.497(6)°, V＝0.66558(19) nm3, Z＝4, Mo Kα, λ＝0.071073 nm, R(F)＝6.00%, wR(F2)＝15.43%. UV-Vis diffu-sion reflectance spectra suggest that the crystals 1 and 2 are semiconductor with estimated band gaps 2.03 and 2.10 eV, respectively. The DSC data show that crystal 1 and crystal 2 collapse at 333 and 352 ℃ respectively, in nitrogen.

Key words: solvothermal synthesis, quaternary thio-tellurite, crystal structure