Transformation of a zinc inclusion complex to wurtzite ZnS microflowers under solvothermal conditions

Transformation of a zinc inclusion complex to wurtzite ZnS microflowers under solvothermal conditions
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DOI:
10.1002/crat.201000291
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发表时间:
2010-09
影响因子:
1.5
通讯作者:
Liwei Mi;Min-Le Han;Zhen Li;Yaming Wang;Changyu Shen;Zhi Zheng
Liwei Mi;Min-Le Han;Zhen Li;Yaming Wang;Changyu Shen;Zhi Zheng
中科院分区:
材料科学4区
文献类型:
--
作者:
Liwei Mi;Min-Le Han;Zhen Li;Yaming Wang;Changyu Shen;Zhi Zheng

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以硫脲和锌包合物为原料,乙二醇(EG)和乙二胺(EN)为溶剂,采用溶剂热法合成了纤锌矿型硫化锌(ZnS)微米花。以氧化锌(ZnO)、4-Cl-3-NH 2-C6 H3 SO 3和桥联配体bipy为配体,在温和条件下合成了包合物{[Zn(bipy)2(H2O)2](4-Cl-3-NH 2-C6 H3 SO 3)2(bipy)(H2O)2}n,其中bipy为4,4 ′-联吡啶,4-Cl-3-NH 2C 6 H3 SO 3 NH为4-氯-3-氨基苯磺酸.通过粉末X射线衍射和元素分析确认了散装产品的相纯度。详细讨论了合成过程中可能影响ZnS产品纯度的因素。结果表明,混合溶剂和起始原料对产物有显著影响。采用X射线单晶衍射、扫描电子显微镜(SEM)、能量色散X射线光谱(EDS)和X射线衍射(XRD)对产物进行表征。(© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA,魏因海姆)
Wurtzite zinc sulfide (ZnS) microflowers were synthesized successfully by a convenient solvothermal route in ethylene glycol (EG) and ethylenediamine (EN) using thiourea and zinc inclusion complex as starting materials. The inclusion complex {[Zn(bipy)2(H2O)2](4‐Cl‐3‐NH2‐C6H3SO3)2(bipy) (H2O)2}n was achieved by the reaction of zinc oxide (ZnO) and 4‐Cl‐3‐NH2‐C6H3SO3 with the bridging ligand bipy under moderate conditions, in which bipy is 4,4′‐bipyridine and 4‐Cl‐3‐NH2C6H3SO3NH is 4‐Chloro‐3‐aminobenzene sulfonic acid. The phase purity of bulk products was confirmed by powder X‐ray diffraction and element analysis. The factors that might affect the purity of the ZnS product during the synthesis were discussed in detail. It was found that the products were significantly affected by the mixed solvents and the starting materials. X‐ray single crystal diffraction, scanning electron microscopy (SEM), energy‐dispersive X‐ray spectrometry (EDS), and X‐ray diffraction (XRD) were used to characterize the products. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)