On the complexity of crystallization of thioantimonates: In-situ energy dispersive X-ray diffraction (EDXRD) studies of the solvothermal formation of the isostructural thioantimonates [TM(tren)Sb_4S_7] (TM = Fe, Zn)

Seidlhofer B.; Antonova E.; Wang J.; Schinkel D.; Bensch W.

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On the complexity of crystallization of thioantimonates: In-situ energy dispersive X-ray diffraction (EDXRD) studies of the solvothermal formation of the isostructural thioantimonates [TM(tren)Sb_4S_7] (TM = Fe, Zn)

机译：关于硫代锑酸盐结晶的复杂性：等结构硫代锑酸盐[TM（tren）Sb_4S_7]（TM = Fe，Zn）的溶剂热形成的原位能量色散X射线衍射（EDXRD）研究

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The formation of the thioantimonates [M(tren)Sb_4S_7] (M = Fe, Zn; tren = tris(2-aminoethyl)amine) has been studied with in-situ energy dispersive X-ray diffraction (EDXRD) under solvothermal conditions. Up to 60 % amine concentration the compound [Fe(tren)Sb_4S_7] coexists with an unknown crystalline material until the end of the reaction. In the concentration range 70-90 % amine the unknown compound and [Fe(tren)Sb _4S_7] are formed at the beginning of the reaction and when the unknown compound starts to disappear a new mixed-valent thioantimonate [Fe(tren)FeSbS_4] nucleates and crystallizes. Using a 100 % tren solution only [Fe(tren)FeSbS_4] could be identified in the powder patterns. The analysis of the data collected under real conditions clearly shows a strong correlation between the disappearance of the unknown compound and the formation of the mixed-valent thioantimonate. Evidences are presented that FeII/FeIII redox reactions play an important role for nucleation and crystal growth of a distinct iron-containing thioantimonate. Because Zn~(2+) is not redox active the formation processes are different and no crystalline intermediate could be detected.

机译：硫代锑酸盐[M（tren）Sb_4S_7]（M = Fe，Zn; tren =三（2-氨基乙基）胺）的形成已在溶剂热条件下用原位能量色散X射线衍射（EDXRD）进行了研究。胺浓度高达60％的化合物[Fe（tren）Sb_4S_7]与未知的结晶物质共存，直到反应结束。在浓度为70-90％的胺中，未知化合物和[Fe（tren）Sb _4S_7]在反应开始时形成，当未知化合物开始消失时，新的混合价硫代锑酸盐[Fe（tren）FeSbS_4]成核并结晶。使用100％的tren溶液只能在粉末图案中鉴定出[Fe（tren）FeSbS_4]。在真实条件下收集的数据分析清楚地表明，未知化合物的消失与混合价硫代锑酸盐的形成之间存在很强的相关性。证据表明，FeII / FeIII氧化还原反应对于独特的含铁硫代锑酸盐的成核和晶体生长起重要作用。由于Zn〜（2+）不具有氧化还原活性，因此形成过程不同，无法检测到任何结晶中间体。

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |2012年第15期|共10页
作者
Seidlhofer B.; Antonova E.; Wang J.; Schinkel D.; Bensch W.;
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正文语种 eng
中图分类化学;
关键词
Crystallization processes; In-situ X-ray diffraction; Solvothermal synthesis; Thioantimonates;

机译：结晶过程;原位X射线衍射;溶剂热合成;硫锑酸盐;

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1. On the complexity of crystallization of thioantimonates: In-situ energy dispersive X-ray diffraction (EDXRD) studies of the solvothermal formation of the isostructural thioantimonates [TM(tren)Sb_4S_7] (TM = Fe, Zn) [J] . Seidlhofer B., Antonova E., Wang J., Zeitschrift fur Anorganische und Allgemeine Chemie . 2012,第15期

机译：关于硫代锑酸盐结晶的复杂性：等结构硫代锑酸盐[TM（tren）Sb_4S_7]（TM = Fe，Zn）的溶剂热形成的原位能量色散X射线衍射（EDXRD）研究
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On the complexity of crystallization of thioantimonates: In-situ energy dispersive X-ray diffraction (EDXRD) studies of the solvothermal formation of the isostructural thioantimonates [TM(tren)Sb_4S_7] (TM = Fe, Zn)

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