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超声化学合成新型纳米棒二维锌(II)配位聚合物;直接热解制备氧化锌纳米粒子。

Sonochemical synthesis of a novel nano-rod two-dimensional zinc(II) coordination polymer; preparation of zinc(II) oxide nanoparticles by direct thermolyses.

机构信息

Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, Tehran, Iran.

出版信息

Ultrason Sonochem. 2011 Mar;18(2):644-51. doi: 10.1016/j.ultsonch.2010.09.017. Epub 2010 Oct 8.

Abstract

A novel mixed-ligand zinc(II) coordination polymer, {Zn(μ-4,4'-bipy)(μ-3-bpdh)(H(2)O)(2)(2)·(4,4'-bipy)(0.5)}(n) (1); 3-bpdh=2,5-bis(3-pyridyl)-3,4-diaza-2,4-hexadiene and 4,4'-bipy=4,4'-bipyridine, has been synthesized and characterized by IR, (1)HNMR and (13)CNMR spectroscopy. The single crystal X-ray data of compound 1 shows that this coordination polymer grows in two dimensions by two different bridging ligands, 4,4'-bipy and 3-bpdh. Also, nano-scale of compound 1 has been synthesized by sonochemical method and characterized by IR, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Thermal stability of compound 1 in single crystalline and nano-scale form was carried out by thermal gravimetric (TG) and differential thermal analysis (DTA). The ZnO nanoparticles were obtained by calcination of compound 1 at 500°C under air atmosphere and by thermolyses in oleic acid at 200°C. The zinc(II) oxide nanoparticles were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM).

摘要

一种新型的混合配体锌(II)配位聚合物,{Zn(μ-4,4'-bipy)(μ-3-bpdh)(H(2)O)(2)(2)·(4,4'-bipy)(0.5)}(n) (1); 3-bpdh=2,5-双(3-吡啶基)-3,4-二氮杂-2,4-己二烯和 4,4'-bipy=4,4'-联吡啶},已经通过红外光谱(IR)、(1)HNMR 和(13)CNMR 光谱法进行了合成和表征。化合物 1 的单晶 X 射线数据表明,这种配位聚合物通过两种不同的桥联配体 4,4'-bipy 和 3-bpdh 在二维方向上生长。此外,通过超声化学法合成了纳米级的化合物 1,并通过红外光谱、X 射线衍射(XRD)和扫描电子显微镜(SEM)进行了表征。通过热重(TG)和差示热分析(DTA)对化合物 1 单晶和纳米级形式的热稳定性进行了研究。通过在空气气氛下将化合物 1 在 500°C 下煅烧以及在 200°C 下在油酸中热解,得到了 ZnO 纳米粒子。通过 X 射线衍射(XRD)和扫描电子显微镜(SEM)对氧化锌纳米粒子进行了表征。

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