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Understanding the role of zinc dithiocarbamate complexes as single source precursors to ZnS nanomaterials
Nanoscale Advances ( IF 4.6 ) Pub Date : 2020/01/09 , DOI: 10.1039/c9na00665f Husn-Ubayda Islam 1, 2 , Anna Roffey 1 , Nathan Hollingsworth 1 , Wim Bras 2, 3 , Gopinathan Sankar 1 , Nora H De Leeuw 4 , Graeme Hogarth 5
Nanoscale Advances ( IF 4.6 ) Pub Date : 2020/01/09 , DOI: 10.1039/c9na00665f Husn-Ubayda Islam 1, 2 , Anna Roffey 1 , Nathan Hollingsworth 1 , Wim Bras 2, 3 , Gopinathan Sankar 1 , Nora H De Leeuw 4 , Graeme Hogarth 5
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Zinc sulfide is an important wide-band gap semi-conductor and dithiocarbamate complexes [Zn(S2CNR2)2] find widespread use as single-source precursors for the controlled synthesis of ZnS nanoparticulate modifications. Decomposition of [Zn(S2CNiBu2)2] in oleylamine gives high aspect ratio wurtzite nanowires, the average length of which was increased upon addition of thiuram disulfide to the decomposition mixture. To provide further insight into the decomposition process, X-ray absorption spectroscopy (XAS) of [Zn(S2CNMe2)2] was performed in the solid-state, in non-coordinating xylene and in oleylamine. In the solid-state, dimeric [Zn(S2CNMe2)2]2 was characterised in accord with the single crystal X-ray structure, while in xylene this breaks down into tetrahedral monomers. In situ XAS in oleylamine (RNH2) shows that the coordination sphere is further modified, amine binding to give five-coordinate [Zn(S2CNMe2)2(RNH2)]. This species is stable to ca. 70 °C, above which amine dissociates and at ca. 90 °C decomposition occurs to generate ZnS. The relatively low temperature onset of nanoparticle formation is associated with amine-exchange leading to the in situ formation of [Zn(S2CNMe2)(S2CNHR)] which has a low temperature decomposition pathway. Combining these observations with the previous work of others allows us to propose a detailed mechanistic scheme for the overall process.
中文翻译：
了解二硫代氨基甲酸锌络合物作为 ZnS 纳米材料单一来源前体的作用
硫化锌是一种重要的宽带隙半导体，二硫代氨基甲酸盐配合物 [Zn(S 2 CNR 2 ) 2 ] 广泛用作单一来源前体，用于 ZnS 纳米颗粒改性的受控合成。 [Zn(S 2 CNBu 2 ) 2 ]在油胺中分解得到高纵横比纤锌矿纳米线，其平均长度在向分解混合物中添加二硫化秋兰姆后增加。为了进一步了解分解过程，在固态、非配位二甲苯和油胺中对[Zn(S 2 CNMe 2 ) 2 ]进行了X射线吸收光谱(XAS)分析。在固态下，二聚体[Zn(S 2 CNMe 2 ) 2 ] 2 的特征与单晶X射线结构一致，而在二甲苯中则分解成四面体单体。油胺(RNH 2 )中的原位XAS表明配位球被进一步修饰，胺结合得到五配位[Zn(S 2 CNMe 2 ) 2 (RNH 2 )]。该物种稳定至约。 70 °C，高于该温度胺解离，约70 °C 时胺解离。90℃分解生成ZnS。纳米颗粒形成的相对低温开始与胺交换相关，导致原位形成[Zn(S 2 CNMe 2 )(S 2 CNHR)]，其具有低温分解途径。将这些观察结果与其他人之前的工作相结合，使我们能够为整个过程提出详细的机制方案。
更新日期：2020-02-19
中文翻译：
了解二硫代氨基甲酸锌络合物作为 ZnS 纳米材料单一来源前体的作用
硫化锌是一种重要的宽带隙半导体，二硫代氨基甲酸盐配合物 [Zn(S 2 CNR 2 ) 2 ] 广泛用作单一来源前体，用于 ZnS 纳米颗粒改性的受控合成。 [Zn(S 2 CNBu 2 ) 2 ]在油胺中分解得到高纵横比纤锌矿纳米线，其平均长度在向分解混合物中添加二硫化秋兰姆后增加。为了进一步了解分解过程，在固态、非配位二甲苯和油胺中对[Zn(S 2 CNMe 2 ) 2 ]进行了X射线吸收光谱(XAS)分析。在固态下，二聚体[Zn(S 2 CNMe 2 ) 2 ] 2 的特征与单晶X射线结构一致，而在二甲苯中则分解成四面体单体。油胺(RNH 2 )中的原位XAS表明配位球被进一步修饰，胺结合得到五配位[Zn(S 2 CNMe 2 ) 2 (RNH 2 )]。该物种稳定至约。 70 °C，高于该温度胺解离，约70 °C 时胺解离。90℃分解生成ZnS。纳米颗粒形成的相对低温开始与胺交换相关，导致原位形成[Zn(S 2 CNMe 2 )(S 2 CNHR)]，其具有低温分解途径。将这些观察结果与其他人之前的工作相结合，使我们能够为整个过程提出详细的机制方案。
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